CN103922738B - La2Zr2O7 transition-layer gradient film structure, preparation and application thereof - Google Patents

La2Zr2O7 transition-layer gradient film structure, preparation and application thereof Download PDF

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CN103922738B
CN103922738B CN201410088329.8A CN201410088329A CN103922738B CN 103922738 B CN103922738 B CN 103922738B CN 201410088329 A CN201410088329 A CN 201410088329A CN 103922738 B CN103922738 B CN 103922738B
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film
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transition layer
precursor liquid
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CN103922738A (en
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索红莉
任程
刘敏
仪宁
田辉
徐燕
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Shenchuang Superconductor Shenzhen Technology Co ltd
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Beijing University of Technology
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Abstract

A La2Zr2O7 transition-layer gradient film structure, preparation and application thereof belong to the technical field of a high-temperature superconductive coating material. According to the La2Zr2O7 transition-layer film provided by the invention, the lower layer is a La2Zr2-xTixO7 film doped with Ti<4+> having small ionic radius, wherein x is less than or equal to 1.8 and greater than or equal to 0.2; and the upper layer is a La2Zr2-yYyO7 film doped with Y<3+> having large ionic radius, wherein y is less than or equal to 1.8 and greater than or equal to 0.2. Through different doping contents, 100% matching between the film and a substrate Ni and a superconducting layer YBCO is realized, and the transition-layer structure of lattice constant gradient change is realized. In addition, the transition layer is the same bulk material and has more stable performance. Lattice constants of the La2Zr2-xTixO7 film and the La2Zr2-yYyO7 film are accurate and adjustable. Integration of multiple transition-layer functions is achieved, and complexity of a present transition-layer structure is minimized.

Description

A kind of La 2zr 2o 7transition layer gradient film structure, preparations and applicatio
Technical field
The invention belongs to high temperature superconducting materia technical field, be specifically related to the technology of preparing of conductor of high-temperature superconductor coat transition layer.
Background technology
Because high temperature superconducting materia YBCO has extremely strong anisotropy, its current capacity is very responsive to lattice mismatch, and large lattice mismatch angle will form Weak link, has a strong impact on its superconductivity.Therefore, need YBCO to be deposited on to have on the metal substrate of biaxial texture.Because YBCO has brittleness of ceramics, in recent years, people adopted on polycrystalline toughness NiW metal base band and deposited superconducting thin film, made its epitaxial substrate texture to obtain the YBCO superconductive film of high orientation.
But because NiW alloy and YBCO superconducting material exist certain lattice mismatch, in addition, NiW alloy also can have stronger diffusion and chemical reaction with YBCO, has a strong impact on YBCO layer superconductivity.Therefore in the middle of NiW alloy and superconducting layer, add one or more layers transition layer film, play the effect of transmitting texture and intercepting Elements Diffusion.
But be difficult to all requirements that a kind of material can meet transition layer, be all that different materials is grouped together as the transition layer structure of coating conductor usually, the structure of current comparative maturity is: CeO 2/ La 2zr 2o 7, CeO 2/ Gd 2zr 2o 7, CeO 2/ YSZ/Y 2o 3deng (as Fig. 1).These transition layer structures comprise cap layer (CeO 2), barrier layer (La 2zr 2o 7, Gd 2zr 2o 7), Seed Layer (Y 2o 3) two or three material, and these materials and Ni, YBCO all have mismatch in various degree.The lattice parameter of Ni is , La 2zr 2o 7lattice lengths corresponding is with it , and the lattice parameter of YBCO .Due to La 2zr 2o 7lattice parameter be greater than the lattice parameter of Ni, adding of Seed Layer is to make it as La 2zr 2o 7nucleating center, improve La 2zr 2o 7the texture degree of transition layer.Again because of CeO 2have high chemical stability, less with the mismatch of YBCO (being only-0.12%), is conducive to YBCO epitaxy, and becomes the top transition layer of deposition YBCO superconducting layer.But multilayer material also cannot adjust the mispairing of Ni and YBCO well, play the effect of transmitting texture; Further, certain Elements Diffusion reaction can also be there is between transition layer, as La 2zr 2o 7with CeO 2, cause texture to reduce; Meanwhile, these transition layer structures are multilayer film, and preparation process is more complicated, and cost is higher, and production efficiency is low, are unfavorable for the application of following large-scale commercial.
In sum, developing single buffer layer material, and adopt chemical solution method preparation with low cost, is focus and the challenge in coating conductor investigation of materials field.This, by greatly simplifying the preparation process of transition layer, enhances productivity, and reduces preparation cost, is beneficial to and advances the business-like process of coating conductor.
Summary of the invention
The object of the invention is to solve Problems existing in existing coating conductor transition layer preparation process, provide a kind of technique simple, efficient, and the with low cost La adulterated with Ti, Y 2zr 2o 7for the gradient film structure (as Fig. 2) of single matrix transition layer.
A kind of La provided by the present invention 2zr 2o 7single transition layer gradient film, is characterized in that, this single transition layer gradient film has double-layer structure, and every layer usually changes La by the unit of the ionic radius varied in size that adulterates 2zr 2o 7lattice parameter, reduce with substrate Ni, superconducting layer YBCO mismatch.Lower floor is the Ti that ionic radius is less 4+the La that doping is formed 2zr 2-xti xo 7film, wherein 0.2≤x≤1.8(preferably 0.8≤x≤1.5), reduce La 2zr 2o 7lattice parameter, reduce La 2zr 2o 7with the mismatch of Ni, lower thickness is preferably 50-150nm; Upper strata is the Y that ionic radius is larger 3+the La that doping is formed 2zr 2-yy yo 7film, 0.2≤y≤1.8(preferably 0.5≤y≤1.2), increase La 2zr 2o 7lattice parameter, reduce La 2zr 2o 7with the mismatch of YBCO, upper thickness is preferably 50-150nm.Can realize mating with the two 100% by adulterating in right amount simultaneously, achieving a kind of transition layer structure of lattice parameter graded.And doping body is commaterial, can not exist as element phase mutual diffusion between above-mentioned multiple buffer layer material, reduces the problem of texture intensity, ensure that the stability of transition layer.
A kind of La 2zr 2o 7the preparation method of single transition layer gradient film, is characterized in that, specifically comprises step as follows:
1) preparation of Ti doping precursor liquid: by titanium acetylacetone and methyl ethyl diketone zirconium, be x:2-x according to the mol ratio of titanium ion and zirconium ion, wherein, 0.2≤x≤1.8(preferably 0.8≤x≤1.5), the total concn of titanium ion and zirconium ion is 0.1-1.0mol/L, be dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Ti doping;
2) preparation of Y doping precursor liquid: by acetic acid yttrium and methyl ethyl diketone zirconium, be y:2-y by the mol ratio of ruthenium ion and zirconium ion, wherein, 0.2≤y≤1.8(preferably 0.5≤y≤1.2), the total concn of titanium ion and zirconium ion is 0.1-1.0mol/L, be dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Y doping;
3) coating of precursor liquid: the mode of precursor liquid spin coating of being adulterated by Ti is coated on Ni substrate, obtains the first layer precursor film;
4) high temperature sintering: at Ar4%H 2under the condition of shielding gas, by precursor film in 950-1200 DEG C of sintering 30-60min, obtain Ti doping La 2zr 2o 7transition layer film;
5) according to step 3) and step 4), the precursor liquid that Y adulterates is carried out be coated to Ti doping La 2zr 2o 7in 950-1200 DEG C of sintering 30-60min on transition layer film, obtain the second layer La of Y doping 2zr 2o 7transition layer.
Application Areas: be applied to YBCO s-generation high temperature coating superconductor, namely at La 2zr 2-yy yo 7film grows YBCO.
The present invention has the following advantages:
1) the transition layer film structure that obtains of the present invention is simple, and a kind of transition layer film achieves the integration of multiple transition layer function, reduces existing complicated transition layer structure.
2) the transition layer film structure that obtains of the present invention, by regulating doping can realize and substrate Ni, 100% mate of superconducting layer YBCO simultaneously, namely adjustment doping makes La 2zr 2-xti xo 7lattice parameter identical with Ni substrate, adjustment doping make La 2zr 2-yy yo 7lattice parameter and growth its on YBCO identical, achieve a kind of transition layer structure of lattice parameter graded.La 2zr 2-xti xo 7, La 2zr 2-yy yo 7film lattice constant is accurately adjustable, and transition layer is same bulk material, thus makes transition layer structure more stable.
3) La that obtains of the present invention 2zr 2-xti xo 7, La 2zr 2-yy yo 7transition layer film lattice parameter is adjustable, thickness can reach 100-300nm, film diaxial orientation grows, cubic texture content reaches more than 90%, surfacing is fine and close, there is the effect intercepting and react to each other between superconducting layer and base material, and the integration of multiple transition layer function can be realized, reduce the complicacy of existing transition layer structure.
Accompanying drawing explanation
Fig. 1. high temperature coating conductor structure schematic diagram;
1 be superconducting layer, 2 be wherein cap layer, 3 be barrier layer, 4 be Seed Layer, 5 for metal substrate layer.
The La of Fig. 2 .Ti, Y doping 2zr 2o 7the gradient film structure of transition layer;
1 is that YBCO layer, 2 is for La 2zr 2-yy yo 7layer, 3 is La 2zr 2-xti xo 7layer, 4 is Ni baseband layer.
Fig. 3. the first layer La after embodiment 1 gained Ti adulterates 2zr 2-xti xo 7the SEM figure of film.
Fig. 4. the second layer La after embodiment 2 gained Y adulterates 2zr 2-yy yo 7(222) face phi scanning curve of film.
Fig. 5. the second layer La after embodiment 3 gained Y adulterates 2zr 2-yy yo 7the pole figure of film.
Fig. 6. the first layer La that embodiment 4 gained Ti adulterates 2zr 2-yy yo 7(004) face psi scanning curve of film.
Specific implementation method
Below in conjunction with the drawings and specific embodiments, the invention will be further described, but the present invention is not limited to following is embodiment.
Embodiment 1
1) preparation of Ti doping precursor liquid: by titanium acetylacetone and methyl ethyl diketone zirconium, be 1:9 according to the mol ratio of titanium ion and zirconium ion, wherein, x=0.2, the total concn of titanium ion and zirconium ion is 0.6mol/L, is dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Ti doping;
2) preparation of Y doping precursor liquid: by acetic acid yttrium and methyl ethyl diketone zirconium, be 2:3 by the mol ratio of ruthenium ion and zirconium ion, wherein, y=0.8, the total concn of titanium ion and zirconium ion is 0.8mol/L, is dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Y doping;
3) coating of precursor liquid: the mode of precursor liquid spin coating of being adulterated by Ti is coated to W metal substrate, obtains the first layer precursor film;
4) high temperature sintering: at Ar4%H 2under the condition of shielding gas, by the first layer precursor film in 950 DEG C of sintering 60min, obtain the Ti doping La that thickness is 100nm 2zr 2o 7transition layer film;
5) according to step 3) and step 4), the precursor liquid that Y adulterates carries out applying by the basis of the first layer film, high temperature sintering, obtain the second layer La that thickness is the Y doping of 100nm 2zr 2o 7transition layer.
The La that embodiment 1 obtains 2zr 2o 7transition layer total thickness is 200nm, the smooth densification of film surface.
Embodiment 2
1) preparation of Ti doping precursor liquid: by titanium acetylacetone and methyl ethyl diketone zirconium, be 1:3 according to the mol ratio of titanium ion and zirconium ion, wherein, x=0.5, the total concn of titanium ion and zirconium ion is 0.6mol/L, is dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Ti doping;
2) preparation of Y doping precursor liquid: by acetic acid yttrium and methyl ethyl diketone zirconium, be 1:1 by the mol ratio of ruthenium ion and zirconium ion, wherein, y=1.0, the total concn of titanium ion and zirconium ion is 1.0mol/L, is dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Y doping;
3) coating of precursor liquid: the mode of precursor liquid spin coating of being adulterated by Ti is coated to W metal substrate, obtains the first layer precursor film;
4) high temperature sintering: at Ar4%H 2under the condition of shielding gas, by precursor film in 1000 DEG C of sintering 40min, obtain the Ti doping La that thickness is 150nm 2zr 2o 7transition layer film;
5) according to step 3) and step 4), the precursor liquid that Y adulterates carries out applying by the basis of the first layer film, high temperature sintering, obtain the second layer La that thickness is the Y doping of 100nm 2zr 2o 7transition layer.
The La that embodiment 2 obtains 2zr 2o 7transition layer total thickness is 250nm, and the face interscan halfwidth in (222) face is 7.55.
Embodiment 3
1) preparation of Ti doping precursor liquid: by titanium acetylacetone and methyl ethyl diketone zirconium, be 1:1 according to the mol ratio of titanium ion and zirconium ion, wherein, x=1.0, the total concn of titanium ion and zirconium ion is 0.8mol/L, is dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Ti doping;
2) preparation of Y doping precursor liquid: by acetic acid yttrium and methyl ethyl diketone zirconium, be 3:2 by the mol ratio of ruthenium ion and zirconium ion, wherein, y=1.2, the total concn of titanium ion and zirconium ion is 0.8mol/L, is dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Y doping;
3) coating of precursor liquid: the mode of precursor liquid spin coating of being adulterated by Ti is coated on metal substrate, obtains the first layer precursor film;
4) high temperature sintering: at Ar4%H 2under the condition of shielding gas, by precursor film in 1100 DEG C of sintering 40min, obtain the Ti doping La that thickness is 100nm 2zr 2o 7transition layer film;
5) according to step 3) and step 4), the precursor liquid that Y adulterates carries out applying by the basis of the first layer film, high temperature sintering, obtain the second layer La that thickness is the Y doping of 200nm 2zr 2o 7transition layer.
The La that embodiment 3 obtains 2zr 2o 7transition layer total thickness is 300nm, and cubic texture content reaches 90%.
Embodiment 4
1) preparation of Ti doping precursor liquid: by titanium acetylacetone and methyl ethyl diketone zirconium, be 9:1 according to the mol ratio of titanium ion and zirconium ion, wherein, x=1.8, the total concn of titanium ion and zirconium ion is 1.0mol/L, is dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Ti doping;
2) preparation of Y doping precursor liquid: by acetic acid yttrium and methyl ethyl diketone zirconium, be 9:1 by the mol ratio of ruthenium ion and zirconium ion, wherein, y=1.8, the total concn of titanium ion and zirconium ion is 1.0mol/L, is dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Y doping;
3) coating of precursor liquid: the mode of precursor liquid spin coating of being adulterated by Ti is coated on W metal substrate, obtains the first layer precursor film;
4) high temperature sintering: at Ar4%H 2under the condition of shielding gas, by precursor film in 1200 DEG C of sintering 30min, obtain the Ti doping La that thickness is 150nm 2zr 2o 7transition layer film;
5) according to step 3) and step 4), the precursor liquid that Y adulterates carries out applying by the basis of the first layer film, high temperature sintering, obtain the second layer La that thickness is the Y doping of 100nm 2zr 2o 7transition layer.
The La that embodiment 4 obtains 2zr 2o 7transition layer total thickness is 250nm, and scanning halfwidth outside the face in (004) face is 10.03.

Claims (6)

1. a La 2zr 2o 7single transition layer gradient film, is characterized in that, this single transition layer gradient film has double-layer structure, and every layer usually changes La by the unit of the ionic radius varied in size that adulterates 2zr 2o 7lattice parameter, lower floor is the Ti that ionic radius is less 4+the La that doping is formed 2zr 2-xti xo 7film, wherein 0.2≤x≤1.8, reduce La 2zr 2o 7lattice parameter; Upper strata is the Y that ionic radius is larger 3+the La that doping is formed 2zr 2-yy yo 7film, 0.2≤y≤1.8, increase La 2zr 2o 7lattice parameter.
2. according to a kind of La of claim 1 2zr 2o 7single transition layer gradient film, is characterized in that, 0.8≤x≤1.5,0.5≤y≤1.2.
3. according to a kind of La of claim 1 2zr 2o 7single transition layer gradient film, is characterized in that, the thickness of lower floor is 50-150nm, and the thickness on upper strata is 50-150nm.
4. prepare a kind of La of claim 1 2zr 2o 7the method of single transition layer gradient film, is characterized in that, comprise step as follows:
1) preparation of Ti doping precursor liquid: by titanium acetylacetone and methyl ethyl diketone zirconium, be x:2-x according to the mol ratio of titanium ion and zirconium ion, wherein, 0.2≤x≤1.8, the total concn of titanium ion and zirconium ion is 0.1-1.0mol/L, be dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Ti doping;
2) preparation of Y doping precursor liquid: by acetic acid yttrium and methyl ethyl diketone zirconium, be y:2-y by the mol ratio of ruthenium ion and zirconium ion, wherein, 0.2≤y≤1.8, the total concn of titanium ion and zirconium ion is 0.1-1.0mol/L, be dissolved in propionic acid, at 40 DEG C of Stirring 30min, obtain the precursor liquid of Y doping;
3) coating of precursor liquid: the mode of precursor liquid spin coating of being adulterated by Ti is coated on Ni substrate, obtains the first layer precursor film;
4) high temperature sintering: at Ar4%H 2under the condition of shielding gas, by precursor film in 950-1200 DEG C of sintering 30-60min, obtain Ti doping La 2zr 2o 7transition layer film;
5) according to step 3) and step 4), the precursor liquid that Y adulterates is carried out be coated to Ti doping La 2zr 2o 7in 950-1200 DEG C of sintering 30-60min on transition layer film, obtain the second layer La of Y doping 2zr 2o 7transition layer.
5. the arbitrary La described in claim 1-3 2zr 2o 7the application of single transition layer gradient film on the YBCO s-generation high temperature coating superconductor substrate Ni is La 2zr 2-xti xo 7film, La 2zr 2-yy yo 7film grows YBCO.
6. according to the La of claim 5 2zr 2o 7the application of single transition layer gradient film on YBCO s-generation high temperature coating superconductor, is characterized in that, by regulating doping to realize and substrate Ni, 100% mate of superconducting layer YBCO simultaneously, namely adjustment doping makes La 2zr 2-xti xo 7lattice parameter identical with Ni substrate, adjustment doping make La 2zr 2-yy yo 7lattice parameter and growth its on YBCO identical.
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