CN104928660B - Superconducting coating YxCe1‑xO2/La2Zr2O7The preparation method of compound transition layer film - Google Patents
Superconducting coating YxCe1‑xO2/La2Zr2O7The preparation method of compound transition layer film Download PDFInfo
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Abstract
The present invention discloses a kind of superconducting coating YxCe1‑xO2/La2Zr2O7The preparation method of compound transition layer film, comprises the following steps：Lanthanum acetate, acetylacetone,2,4-pentanedione zirconium, propionic acid are dissolved in methanol solvate, La is obtained2Zr2O7Precursor aqueous solution；By acetic acid yttrium, cerous acetate is dissolved in containing propionic acid, in the methanol solvate of acetylacetone,2,4-pentanedione, obtains YxCe1‑xO2Precursor aqueous solution.Using solution film plating process, La is prepared on the flexible nickel-tungsten alloy base-band with biaxial texture2Zr2O films, and YxCe1‑xO2Film, forms YxCe1‑xO2/La2Zr2O7Composite coating.The present invention combines the La that can effectively hinder YBCO and Ni to spread2Zr2O7As bottom, and with the Y with YBCO lattice comparison matchxCe1‑xO2As top layer, film has good surface smoothness and c-axis orientation, and avoids CeO2Film is easy to the shortcoming of cracking.
Description
Technical field
The present invention relates to high-temperature superconducting thin film cushion preparing technical field.More particularly to a kind of superconducting coating YxCe1- xO2/La2Zr2O7The preparation method of compound transition layer film.
Background technology
High-temperature superconducting thin film or coating have broad application prospects in field of power electronics.It is high in field of power transmission
Temperature superconductive technology is the important high-tech technology of 21 century power domain.For power domain, in flexible NiW metal base bands
The YBa of upper preparation2Cu3O7-x（YBCO）High-temperature superconducting coating, with very great development potentiality, but still needs in flexible NiW metals
One layer of transition zone is prepared in substrate.
These transition zones serve very crucial effect, not only can provide basis for the growth of YBCO coatings, moreover it is possible to
Diffusion between barrier metal Ni and superconducting layer YBCO.These transition zones include：CeO2, La2Zr2O7, SrTiO3Etc..And how
These transition zones are prepared, multiple technologies are further related to, including：Magnetron sputtering（MS）, pulsed laser deposition（PLD）, metal is organic
Thing chemical vapor deposition（MOCVD）, deposition of metal organic（MOD）And sol-gel（sol-gel）.Wherein MS, PLD,
MOCVD etc. needs vacuum facility, and equipment is expensive, and the preparation cost of film or coating is higher.And deposition of metal organic（MOD）With
Sol-gel（sol-gel）It without vacuum facility, need to only depress, you can complete the preparation of film, and have in 1 normal atmosphere
Equipment is simple, the characteristics of cost is low.Therefore, current Many researchers or engineers and technicians have put into more energy and used
MOD/sol-gel technologies develop CeO2, La2Zr2O7, SrTiO3Deng the preparation of transition zone.
CeO2It is good buffer layer material with the lattice match good with YBCO crystal.But ceria film compared with
Easily cracking is produced when thick, it is necessary to introduce rare earth element and be doped, could effectively solve this problem.In addition, CeO2Transition
When growing YBCO superconductive film on layer, it also occur that Ce and Ba chemical reaction, forms BaCeO3Dephasign.These are all current
CeO2The problem of transition zone needs to solve.Importantly, CeO2Transition zone can not effectively obstruct the diffusion between YBCO and Ni,
Therefore also tend to constitute compound transition zone together with other transition zones and could obtain high performance YBCO coatings.
In recent years, substantial amounts of researcher develops La2Zr2O7Transition zone, it is desirable to taken in Ni and deposited rear La2Zr2O7
Transition zone, directly prepares YBCO coatings.But result shows, in La2Zr2O7Often performance is unsatisfactory for the YBCO coatings of upper preparation.
The YBCO prepared especially with chemical method, easily forms a axialites grain.
Therefore, for the chemical preparation YBCO coating conductors of low cost, using single CeO2Transition zone, or it is single
La2Zr2O7Transition zone, can not all meet the requirement of high-performance Y BCO coatings.Design and prepare a kind of new compound transition
Layer is significant.The invention provides a kind of compound transition layer structure, the CeO that Y is adulterated2, i.e. YxCe1-xO2Film, with
La2Zr2O7Film laminated, by controlling the number of plies and thickness of coating, obtains high performance YxCe1-xO2/La2Zr2O7Compound transition
Layer, is that high performance YBCO coatings preparation is laid a good foundation.
The content of the invention
It is an object of the invention to provide a kind of superconducting coating YxCe1-xO2/La2Zr2O7The method of compound transition layer film,
The superconducting coating Y that this preparation method is obtainedxCe1-xO2Transition layer film is employed can grow the Y for providing growth templates for YBCO
The CeO of doping2Film（YxCe1-xO2）As cap layer, with reference to the La that can effectively hinder YBCO and Ni to spread2Zr2O7It is used as bottom
Layer, so as to form YxCe1-xO2/La2Zr2O7Compound transition zone, by controlling solution concentration, Technology for Heating Processing, the film number of plies,
Obtain that thickness is controllable, the stable compound transition zone of performance, obtained YxCe1-xO2Film has good surface smoothness and c
Axle is orientated, and avoids CeO2Film is easy to the shortcoming of cracking.
To achieve the above object of the invention, the technical solution adopted by the present invention is：A kind of superconducting coating YxCe1-xO2/
La2Zr2O7The method of compound transition layer film, comprises the following steps：
Step 1: lanthanum acetate, acetylacetone,2,4-pentanedione zirconium, propionic acid are dissolved in methanol solvate, La is obtained2Zr2O7Precursor aqueous solution,
This La2Zr2O7Mol ratio is lanthanum acetate in precursor aqueous solution：Acetylacetone,2,4-pentanedione zirconium：Propionic acid=1：1：6；
Step 2: YxCe1-xO2The preparation of precursor aqueous solution, acetic acid yttrium is dissolved in the methanol solvate containing propionic acid, is obtained
Acetic acid yttrium, propionic acid mol ratio are 1 in yttrium solution, this yttrium solution：6；Cerous acetate is dissolved in the first containing acetylacetone,2,4-pentanedione and propionic acid
In alcoholic solvent, it is 1 to obtain cerous acetate, acetylacetone,2,4-pentanedione and propionic acid mol ratio in cerium solution, this cerium solution：4：8；
Step 3: yttrium solution and cerium solution are mixed, Y is obtainedxCe1-xO2Precursor aqueous solution, the YxCe1-xO2In precursor aqueous solution
Yttrium：Cerium=x：（1-x）, wherein x=0.1-0.3；
Step 4: by dip-coating method or spin coating method, in the flexible nickel-tungsten alloy base-band with biaxial texture
Upper coating La2Zr2O7Precursor aqueous solution formation La2Zr2O7Gel film layer；
Step 5: by La2Zr2O7Gel film layer dries 15 ~ 20min at a temperature of 100 ~ 180 DEG C, obtains La2Zr2O7
Dry film, then by La2Zr2O7Dry film is put into quartz tube type sintering furnace, under the conditions of the first protective atmosphere, with 15 DEG C/min's
In-furnace temperature is increased to after 250 DEG C, insulation 10min by speed, continues to be warming up to 1050 DEG C, and atmosphere is switched into the second protection
Atmosphere, continues to be incubated 60min, after insulation terminates, cools to room temperature with the furnace under the second protective atmosphere, obtaining has La2Zr2O7
The substrate of film；
Step 6: by dip-coating method or spin coating method, being made in step 5 has La2Zr2O7The substrate of film
La2Zr2O7Film surface coats YxCe1-xO2Gel film layer, by YxCe1-xO2Gel film layer is at a temperature of 100 ~ 180 DEG C
15 ~ 20min is dried, Y is obtainedxCe1-xO2Gel dry film；
Step 7: again by YxCe1-xO2Gel dry film is put into quartz tube type sintering furnace, under the conditions of the second protective atmosphere,
In-furnace temperature is increased to after 250 DEG C, insulation 10min with 15 DEG C/min speed, continues to be warming up to 950 ~ 1050 DEG C, and be incubated
60min, after insulation terminates, cools to room temperature with the furnace.
Further improved technology scheme is as follows in above-mentioned technical proposal：
1. in such scheme, La prepared by the step one2Zr2O7In precursor aqueous solution, La and the total concentration of metal ions of Zr
Control is in 0.25 ~ 0.3mol/l.
2. in such scheme, Y prepared by the step 3xCe1-xO2In precursor aqueous solution, Y and the total concentration of metal ions controls of Ce
System is in 0.2 ~ 0.25mol/l.
3. it is described Step 4: the La of step 5 in such scheme2Zr2O7The preparation process of film is alternately repeated 2 ~ 3 times,
To obtain 2 ~ 3 layers of La2Zr2O7Film.
4. in such scheme, the step 5 La2Zr2O7First protective atmosphere of the preparation process of film is H2、CO2
And N2Mixed atmosphere, wherein, hydrogen content 5 ~ 6vol.%, CO2Content is 3 ~ 7vol.%, N2Content is 89 ~ 92vol.%；Step
Five La2Zr2O7The preparation process and step 7 Y of filmxCe1-xO2Second protective atmosphere described in the preparation process of film is H2With
N2Mixed atmosphere, wherein, hydrogen content 5 ~ 6vol.%, N2Content is 85 ~ 94vol.%.
5. it is described Step 6: the Y of step 7 in such schemexCe1-xO2The preparation process of film is alternately repeated 2 ~ 3 times,
To obtain 2 ~ 3 layers of YxCe1-xO2Film.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
1. a kind of superconducting coating Y of the inventionxCe1-xO2/La2Zr2O7The method of compound transition layer film, instead of tradition
CeO2Film and its technology of preparing, pass through Y made from chemical methodxCe1-xO2There is film good surface smoothness and c-axis to take
To, and avoid CeO2Film is easy to the shortcoming of cracking.
2. preparation method of the present invention is by YxCe1-xO2With La2Zr2O7Film laminated, the compound transition zone of formation is not only avoided
Single CeO2Film or YxCe1-xO2YBCO and Ni diffusion problem can not be effectively obstructed, single La is it also avoid2Zr2O7Film
The problem of c-axis YBCO grain growths can not effectively be induced.
3. by controlling La in preparation method of the present invention2Zr2O7Precursor aqueous solution ion concentration（0.25-0.3mol/l）, make
Obtain prepared La2Zr2O7Film is entirely c-axis orientation, for induction YxCe1-xO2Oriented growth lay a good foundation；Meanwhile, lead to
Cross control YxCe1-xO2Precursor aqueous solution ion concentration（0.2-0.25mol/l）So that prepared YxCe1-xO2Film is entirely c
Axle is orientated, to induce YBCO oriented growth to lay a good foundation.On the basis of concentration is controlled, transition zone is further controlled
The number of plies, and then the thickness of film is controlled, so as to effectively achieve barriering effect.
4. a kind of superconducting coating Y of the inventionxCe1-xO2/La2Zr2O7The method of compound transition layer film, in La2Zr2O7
Film is employed containing CO in heat treatment process2, N2, and H2Atmosphere, the CO in the atmosphere2Can be with the residual C in film
React and generate CO, the C residuals in film are taken away, so as to improve the consistency and texture degree of film.Meanwhile, the N in the atmosphere2
And H2, metal base band can be prevented to be oxidized, played a protective role.So, the consistency of film is not only increased, it is therefore prevented that substrate
Oxidation, also helps the raising of film c-axis texture degree, and it is loose to solve existing transition layer film, the defect such as texture degree difference, meets
The application of conductor of high-temperature superconductor coat.
Brief description of the drawings
2 layers of La that accompanying drawing 1 is prepared for the present invention on Ni2Zr2O7The XRD of film；
Accompanying drawing 2 is Y of the present inventionxCe1-xO2/La2Zr2O7The XRD of compound transition layer film；
Accompanying drawing 3 is Y of the present inventionxCe1-xO2/La2Zr2O7Compound transition layer film（111）The XRD-phi scanning figures in face；
Accompanying drawing 4 is Y of the present inventionxCe1-xO2/La2Zr2O7The atomic force surface topography map of compound transition layer film；
Accompanying drawing 5 is Y of the present inventionxCe1-xO2/La2Zr2O7The superconductivity figure of the ybco film prepared on compound transition zone.
Embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1：A kind of superconducting coating YxCe1-xO2/La2Zr2O7The chemical solution preparation method of compound transition zone, bag
Include following steps：
Step 1: La2Zr2O7The preparation of precursor aqueous solution.Preparation process is：By lanthanum acetate, acetylacetone,2,4-pentanedione zirconium, propionic acid dissolving
In methanol solvate, you can obtain La2Zr2O7Precursor aqueous solution.Mol ratio lanthanum acetate in solution：Acetylacetone,2,4-pentanedione zirconium：Propionic acid=1：1：
6.By the consumption for adjusting methanol solvate so that total concentration of metal ions in solution is 0.3mol/l.
Step 2: Y0.2Ce0.8O2The preparation of precursor aqueous solution, comprises the following steps（1）Acetic acid yttrium is dissolved in containing propionic acid
In methanol solvate, yttrium solution is obtained.In the solution, acetic acid yttrium：Propionic acid=1:6；（2）Cerous acetate be dissolved in containing acetylacetone,2,4-pentanedione and
In the methanol solvate of propionic acid, cerium solution is obtained.In the solution, cerous acetate：Acetylacetone,2,4-pentanedione：Propionic acid=1:4：8.(3) by yttrium solution
With the mixing of cerium solution, Y is obtained0.2Ce0.8O2Precursor aqueous solution.In the solution, yttrium：Cerium=0.2:0.8. by adjusting methanol solvate
Consumption so that total concentration of metal ions in solution is 0.25mol/l.
Step 3: La2Zr2O7The preparation of film.Preparation process is：（1）By dip-coating method or spin coating method,
La is coated on the flexible nickel-tungsten alloy base-band with biaxial texture2Zr2O7Gel film layer；（2）By gel film layer 100 ~ 180
15 ~ 20min is dried at a temperature of DEG C, La is obtained2Zr2O7Dry film；（3）By La2Zr2O7Dry film is put into quartz tube type sintering furnace,
Under the conditions of the first protective atmosphere, in-furnace temperature is increased to after 250 DEG C, insulation 10min with 15 DEG C/min speed, continued
1050 DEG C are warming up to, and atmosphere is switched into the second protective atmosphere, continues to be incubated 60min.After insulation terminates, gas is protected second
Cool to room temperature under atmosphere with the furnace, obtain La2Zr2O7Film.
Above-mentioned plated film and heat treatment process are carried out 2 times altogether, to obtain 2 layers of La2Zr2O7Film, can finally be obtained
La2Zr2O7/ NiW transition layer films.
Step 4: Y0.2Ce0.8O2The preparation of film.Preparation process is：（1）By dip-coating method or spin coating method,
With La made from step 32Zr2O7/ NiW films are substrate, coat YxCe1-xO2Gel film layer；（2）By gel film layer 100 ~
15 ~ 20min is dried at a temperature of 180 DEG C, Y is obtainedxCe1-xO2Gel dry film；（3）By YxCe1-xO2Gel dry film is put into quartz ampoule
In formula sintering furnace, under the conditions of the second protective atmosphere, in-furnace temperature is increased to by 250 DEG C, insulation with 15 DEG C/min speed
After 10min, continue to be warming up to 950 DEG C, and be incubated 60min.After insulation terminates, room temperature is cooled to the furnace.
Above-mentioned plated film and heat treatment process are carried out 2 times altogether, to obtain 2 layers of Y0.2Ce0.8O2Film, it is final to obtain
Y0.2Ce0.8O2/La2Zr2O7/ NiW is combined transition layer film.
Above-mentioned steps three, the first protective atmosphere described in step 4 is H2、CO2And N2Mixed atmosphere, wherein, hydrogen
Content 5 ~ 6vol.%, CO2Content is 3 ~ 7vol.%, N2Content is 89 ~ 92vol.%.The second protective atmosphere described in step 3 is
H2And N2Mixed atmosphere, wherein, hydrogen content 5 ~ 6vol.%, N2Content is 85 ~ 94vol.%.
Embodiment 2：A kind of superconducting coating YxCe1-xO2/La2Zr2O7The chemical solution preparation method of compound transition zone, bag
Include following steps：
Step 1: La2Zr2O7The preparation of precursor aqueous solution.Preparation process is：By lanthanum acetate, acetylacetone,2,4-pentanedione zirconium, propionic acid dissolving
In methanol solvate, you can obtain La2Zr2O7Precursor aqueous solution.Mol ratio lanthanum acetate in solution：Acetylacetone,2,4-pentanedione zirconium：Propionic acid=1：1：
6.By the consumption for adjusting methanol solvate so that total concentration of metal ions in solution is 0.25mol/l.
Step 2: Y0.1Ce0.9O2The preparation of precursor aqueous solution, comprises the following steps（1）Acetic acid yttrium is dissolved in containing propionic acid
In methanol solvate, yttrium solution is obtained.In the solution, acetic acid yttrium：Propionic acid=1:6；（2）Cerous acetate be dissolved in containing acetylacetone,2,4-pentanedione and
In the methanol solvate of propionic acid, cerium solution is obtained.In the solution, cerous acetate：Acetylacetone,2,4-pentanedione：Propionic acid=1:4：8.(3) by yttrium solution
With the mixing of cerium solution, Y is obtainedxCe1-xO2Precursor aqueous solution.In the solution, yttrium：Cerium=0.3:0.7. by adjusting the use of methanol solvate
Amount so that total concentration of metal ions in solution is 0.2mol/l.
Step 3: La2Zr2O7The preparation of film.Preparation process is：（1）By dip-coating method or spin coating method,
La is coated on the flexible nickel-tungsten alloy base-band with biaxial texture2Zr2O7Gel film layer；（2）By gel film layer 100 ~ 180
15 ~ 20min is dried at a temperature of DEG C, La is obtained2Zr2O7Dry film；（3）By La2Zr2O7Dry film is put into quartz tube type sintering furnace,
Under the conditions of the first protective atmosphere, in-furnace temperature is increased to after 250 DEG C, insulation 10min with 15 DEG C/min speed, continued
1050 DEG C are warming up to, and atmosphere is switched into the second protective atmosphere, continues to be incubated 60min.After insulation terminates, gas is protected second
Cool to room temperature under atmosphere with the furnace, obtain La2Zr2O7Film.
Above-mentioned plated film and heat treatment process are carried out 2 times altogether, to obtain 2 layers of La2Zr2O7Film, can finally be obtained
La2Zr2O7/ NiW transition layer films.
Step 4: YxCe1-xO2The preparation of film.Preparation process is：（1）By dip-coating method or spin coating method, with
La made from step 32Zr2O7/ NiW films are substrate, coat YxCe1-xO2Gel film layer；（2）By gel film layer 100 ~ 180
15 ~ 20min is dried at a temperature of DEG C, Y is obtainedxCe1-xO2Gel dry film；（3）By YxCe1-xO2Gel dry film is put into quartz tube type
In sintering furnace, under the conditions of the second protective atmosphere, in-furnace temperature is increased to 250 DEG C with 15 DEG C/min speed, 10min is incubated
Afterwards, continue to be warming up to 950 DEG C, and be incubated 60min.After insulation terminates, room temperature is cooled to the furnace.
Above-mentioned plated film and heat treatment process are carried out 3 times altogether, to obtain 3 layers of YxCe1-xO2Film, finally obtains YxCe1-xO2/
La2Zr2O7/ NiW is combined transition layer film.
Above-mentioned steps three, the first protective atmosphere described in step 4 is H2、CO2And N2Mixed atmosphere, wherein, hydrogen
Content 5 ~ 6vol.%, CO2Content is 3 ~ 7vol.%, N2Content is 89 ~ 92vol.%.The second protective atmosphere described in step 3 is
H2And N2Mixed atmosphere, wherein, hydrogen content 5 ~ 6vol.%, N2Content is 85 ~ 94vol.%.
Embodiment 3：A kind of superconducting coating YxCe1-xO2/La2Zr2O7The chemical solution preparation method of compound transition zone, bag
Include following steps：
Step 1: La2Zr2O7The preparation of precursor aqueous solution.Preparation process is：By lanthanum acetate, acetylacetone,2,4-pentanedione zirconium, propionic acid dissolving
In methanol solvate, you can obtain La2Zr2O7Precursor aqueous solution.Mol ratio lanthanum acetate in solution：Acetylacetone,2,4-pentanedione zirconium：Propionic acid=1：1：
6.By the consumption for adjusting methanol solvate so that total concentration of metal ions in solution is 0.25mol/l.
Step 2: YxCe1-xO2The preparation of precursor aqueous solution, comprises the following steps（1）Acetic acid yttrium is dissolved in the first containing propionic acid
In alcoholic solvent, yttrium solution is obtained.In the solution, acetic acid yttrium：Propionic acid=1:6；（2）Cerous acetate is dissolved in containing acetylacetone,2,4-pentanedione and third
In the methanol solvate of acid, cerium solution is obtained.In the solution, cerous acetate：Acetylacetone,2,4-pentanedione：Propionic acid=1:4：8.(3) by yttrium solution and
Cerium solution is mixed, and obtains YxCe1-xO2Precursor aqueous solution.In the solution, yttrium：Cerium=0.1:0.9. by adjusting the use of methanol solvate
Amount so that total concentration of metal ions in solution is 0.2mol/l.
Step 3: La2Zr2O7The preparation of film.Preparation process is：（1）By dip-coating method or spin coating method,
La is coated on the flexible nickel-tungsten alloy base-band with biaxial texture2Zr2O7Gel film layer；（2）By gel film layer 100 ~ 180
15 ~ 20min is dried at a temperature of DEG C, La is obtained2Zr2O7Dry film；（3）By La2Zr2O7Dry film is put into quartz tube type sintering furnace,
Under the conditions of the first protective atmosphere, in-furnace temperature is increased to after 250 DEG C, insulation 10min with 15 DEG C/min speed, continued
1050 DEG C are warming up to, and atmosphere is switched into the second protective atmosphere, continues to be incubated 60min.After insulation terminates, gas is protected second
Cool to room temperature under atmosphere with the furnace, obtain La2Zr2O7Film.
Above-mentioned plated film and heat treatment process are carried out 3 times altogether, to obtain 3 layers of La2Zr2O7Film, can finally be obtained
La2Zr2O7/ NiW transition layer films.
Step 4: YxCe1-xO2The preparation of film.Preparation process is：（1）By dip-coating method or spin coating method, with
La made from step 32Zr2O7/ NiW films are substrate, coat YxCe1-xO2Gel film layer；（2）By gel film layer 100 ~ 180
15 ~ 20min is dried at a temperature of DEG C, Y is obtainedxCe1-xO2Gel dry film；（3）By YxCe1-xO2Gel dry film is put into quartz tube type
In sintering furnace, under the conditions of the second protective atmosphere, in-furnace temperature is increased to 250 DEG C with 15 DEG C/min speed, 10min is incubated
Afterwards, continue to be warming up to 1050 DEG C, and be incubated 60min.After insulation terminates, room temperature is cooled to the furnace.
Above-mentioned plated film and heat treatment process are carried out 2 times altogether, to obtain 2 layers of YxCe1-xO2Film, finally obtains YxCe1-xO2/
La2Zr2O7/ NiW is combined transition layer film.
Above-mentioned steps three, the first protective atmosphere described in step 4 is H2、CO2And N2Mixed atmosphere, wherein, hydrogen
Content 5 ~ 6vol.%, CO2Content is 3 ~ 7vol.%, N2Content is 89 ~ 92vol.%.The second protective atmosphere described in step 3 is
H2And N2Mixed atmosphere, wherein, hydrogen content 5 ~ 6vol.%, N2Content is 85 ~ 94vol.%.
The XRD for 2 layers of La2Zr2O7 films that accompanying drawing 1 is prepared for the present invention on Ni, it can be seen that first
The La2Zr2O7 prepared under protective atmosphere and the second protective atmosphere has complete c-axis orientation diffraction maximum, is deposited without other diffraction maximums
；
Accompanying drawing 2 is Y of the present inventionxCe1-xO2/La2Zr2O7The XRD of compound transition layer film；It can be seen that made
Standby YxCe1-xO2/La2Zr2O7Compound transition layer film has complete c-axis orientation diffraction maximum, exists without other diffraction maximums；
Accompanying drawing 3 is Y of the present inventionxCe1-xO2/La2Zr2O7Compound transition layer film（111）The XRD-phi scanning figures in face；In figure
Four axial symmetry are distributed, and illustrate that compound transition layer film has in good face and are orientated；
Accompanying drawing 4 is Y of the present inventionxCe1-xO2/La2Zr2O7The atomic force surface topography map of compound transition layer film, surfacing
Smooth, roughness only has 2.2nm or so；
Accompanying drawing 5 is Y of the present inventionxCe1-xO2/La2Zr2O7The superconductivity figure of the ybco film prepared on compound transition zone,
Film has the critical transition temperature higher than 90K, and temperature transition span only has Δ T=90.6-90.2=0.4K, illustrates that film has
There is good superconductivity.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent change or modification that Spirit Essence is made, should all be included within the scope of the present invention.
Claims (3)
1. a kind of superconducting coating YxCe1-xO2/La2Zr2O7The preparation method of compound transition layer film, it is characterised in that：Including with
Lower step：
Step 1: lanthanum acetate, acetylacetone,2,4-pentanedione zirconium, propionic acid are dissolved in methanol solvate, La is obtained2Zr2O7Precursor aqueous solution, this
La2Zr2O7Mol ratio is lanthanum acetate in precursor aqueous solution：Acetylacetone,2,4-pentanedione zirconium：Propionic acid=1：1：6；
Step 2: YxCe1-xO2The preparation of precursor aqueous solution, acetic acid yttrium is dissolved in the methanol solvate containing propionic acid, obtains yttrium molten
Acetic acid yttrium, propionic acid mol ratio are 1 in liquid, this yttrium solution：6；Cerous acetate is dissolved in the methanol containing acetylacetone,2,4-pentanedione and propionic acid molten
In agent, it is 1 to obtain cerous acetate, acetylacetone,2,4-pentanedione and propionic acid mol ratio in cerium solution, this cerium solution：4：8；
Step 3: yttrium solution and cerium solution are mixed, Y is obtainedxCe1-xO2Precursor aqueous solution, the YxCe1-xO2Yttrium in precursor aqueous solution：Cerium=
x：（1-x）, wherein x=0.1-0.3；
Step 4: by dip-coating method or spin coating method, being applied on the flexible nickel-tungsten alloy base-band with biaxial texture
Cover La2Zr2O7Precursor aqueous solution formation La2Zr2O7Gel film layer；
Step 5: by La2Zr2O7Gel film layer dries 15 ~ 20min at a temperature of 100 ~ 180 DEG C, obtains La2Zr2O7It is dry
Film, then by La2Zr2O7Dry film is put into quartz tube type sintering furnace, under the conditions of the first protective atmosphere, with 15 DEG C/min speed
In-furnace temperature is increased to after 250 DEG C, insulation 10min by rate, continues to be warming up to 1050 DEG C, and atmosphere is switched into the second protection gas
Atmosphere, continues to be incubated 60min, after insulation terminates, cools to room temperature with the furnace under the second protective atmosphere, obtaining has La2Zr2O7It is thin
The substrate of film；
Step 6: by dip-coating method or spin coating method, being made in step 5 has La2Zr2O7The substrate of film
La2Zr2O7Film surface coats YxCe1-xO2Gel film layer, by YxCe1-xO2Gel film layer is at a temperature of 100 ~ 180 DEG C
15 ~ 20min is dried, Y is obtainedxCe1-xO2Gel dry film；
Step 7: again by YxCe1-xO2Gel dry film is put into quartz tube type sintering furnace, under the conditions of the second protective atmosphere, with 15
DEG C/in-furnace temperature is increased to after 250 DEG C, insulation 10min by min speed, continue to be warming up to 950 ~ 1050 DEG C, and be incubated
60min, after insulation terminates, cools to room temperature with the furnace；La prepared by the step one2Zr2O7In precursor aqueous solution, La and Zr are always golden
Belong to ion concentration control in 0.25 ~ 0.3mol/l；Y prepared by the step 3xCe1-xO2In precursor aqueous solution, Y and the total metals of Ce from
Sub- concentration control is in 0.2 ~ 0.25mol/l.
2. a kind of superconducting coating Y according to claim 1xCe1-xO2/La2Zr2O7The method of compound transition layer film, its
It is characterised by：It is described Step 4: the La of step 52Zr2O7The preparation process of film is alternately repeated 2 ~ 3 times, to obtain 2 ~ 3 layers
La2Zr2O7Film.
3. a kind of superconducting coating Y according to claim 1xCe1-xO2/La2Zr2O7The method of compound transition layer film, its
It is characterised by：It is described Step 6: the Y of step 7xCe1-xO2The preparation process of film is alternately repeated 2 ~ 3 times, to obtain 2 ~ 3 layers
YxCe1-xO2Film.
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