MOCVD法制备REBCO超导厚膜及多层膜夹层材料的结构和性能研究
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摘要
提高超导膜的电流承载能力是目前高温超导强电应用方面亟需解决的问题，而临界电流的大小主要由超导膜的厚度（d）和临界电流密度（Jc）决定，因此，要获得较大的电流承载的能力需要从超导膜厚度的增加和钉扎中心的引入两个方面寻求突破。本论文基于光辅助MOCVD技术，围绕这两个方面问题开展了高结晶质量REBCO超导厚膜及多层膜中间夹层材料的制备与性能研究。
本论文采用光辅助MOCVD技术制备出了具有类单晶形貌，良好晶体结构，高临界电流密度的YBCO薄膜，J_c最高达到3.75MA/cm~2，详细分析了衬底生长温度，源挥发比例对薄膜形貌、结晶质量及超导性能的影响。以优化后的工艺条件为基础制备了高质量的YBCO厚膜，并研究了由于薄膜厚度增加所引起的薄膜性质的一些变化。
作为多层膜结构研究的前期准备工作，首次选用GdBCO作为以后研究多层膜结构的夹层材料。并首次采用光辅助MOCVD技术制备出了纯的GdBCO外延膜，研究了衬底温度、氧分压、组分等工艺条件对外延膜晶体质量、生长速率、超导性能的影响。系统的分析了不同厚度薄膜制备过程中薄膜的生长速率、微结构变化和应力释放现象，以及它们对薄膜的晶体质量和超导性质的影响。
选用了Y_2O_3纳米薄层结构作为另一种中间夹层材料。首次利于光辅助MOCVD技术在图形化衬底上进行了应力诱导Y_2O_3纳米薄层结构的自组装生长，并研究了制备过程中的热力学和成核动力学过程。利用高温热处理衬底产生的原子级晶格台阶实现了对Y_2O_3纳米结构在空间分布上的控制。从热力学的角度出发，研究了生长温度和氧分压对Y_2O_3纳米薄层结构生长的影响，并利用两种动力学过程的竞争机制对生长机理进行了分析。从生长动力学角度，研究了生长时间和退火处理时间对于Y_2O_3纳米结构生长的影响。
To improve the current carrying capacity of the superconducting film is an increasinglyurgent need for power applications of high-temperature superconductors. The value ofcritical current depends on the film thickness (d) and the critical current density (Jc). It iswell known that the critical current density of pure YBa_2Cu_3O_(7-δ)(YBCO) films can becomevery high due to a number of growth-induced structural defects such as dislocations. Forpractical applications, however, the flux pinning still needs to be further improved toovercome the vortex motion at high magnetic fields. Therefore, to obtain a larger currentcarrying capacity needs to seek a breakthrough in the thickness of the superconducting filmand the pinning centers. In this paper, photo-assisted metal organic chemical vapordeposition (MOCVD) epitaxial system was employed to fabricate REBCO high quality thickfilms and interlayers of multilayer structure, and their structure and properties wereinvestigated.
In this paper, high-quality YBCO epitaxial films were grown by a photo-assistedMOCVD technique, the films with single-crystal-like morphology, high crystalline andsuperconductive quality were characterized. The highest value of Jcis3.75MA cm~(-2)at77Kin self-field. The effects of substrate temperature and precursors’ proportion on morphology,crystallographic and superconductive quality were investigated. Base on the optimizedprocess conditions, high-quality YBCO thick films was fabricated by controlling thedeposition time. The reason why epitaxial YBCO thick films with high-qualitysingle-crystal-like morphology can be grown up to about2.1μm thick is illustrated from the point of view of photo activation. Meanwhile, the evaluation of film properties with variousthicknesses was systematically investigated. Therefore, the PhA-MOCVD technique mayprovide some advantages for high-rate growth of high-quality YBCO thick films over otherdeposition techniques for various important applications.
As the preliminary preparation for the research of multilayer structure, GdBa_2Cu_3O_7-δ(GdBCO) was firstly used as the interlayer. Photo-assisted MOCVD was employed tofabricate pure GdBCO films for the first time. The effects of substrate temperature (Ts) andoxygen partial pressure (PO2) on microstructure, growth rate and superconducting criticalcurrent density (Jc) were investigated. The (001) preferred orientation of the GdBCO filmswas enhanced with increasing Ts. Film growth rate and degree of texture were found to beinfluenced by PO2. The highly c-axis oriented GdBCO film with Jcof2.5MA/cm~2at77K inself-field was obtained at Tsof810°C and PO_2of4Torr, and the morphology of GdBCOfilm was characterized as single-crystal-like. A growth rate of0.107μm/min is realized bythe PhA-MOCVD technique.
High-quality GdBCO films with thicknesses of0.14-1.62μm were fabricated byPhA-MOCVD technique. Evaluation of film microstructure and strain-relaxationphenomenon in the growing films, and their effects on the crystallographic andsuperconducting properties of the GdBCO films were investigated. A dense and no grainboundary visible, single-crystal-like cross-sectional morphology was observed. For a0.31μm GdBCO film sample, the full width at half-maximum were0.08°and0.47°forout-of-plane and in-plane orientations, respectively. To our knowledge, this is the best valuereported to date for GdBCO heteroepitaxial films, which demonstrate that the films possesswell biaxial texture. The c-axis lattice parameters of the GdBCO films grown with differentthicknesses were used to determine the out-of-plane strain. The result shows that the straincould be gradually relieved as film thickness increasing. As films were getting thicker, theirJcvalues decrease gradually. This is mainly attributed to a lack of pinning centers in thethicker films.
We choose Y_2O_3nano thin film structure as another interlayer for the study of multilayer structure in future. Self-assembling of strain-induced Y_2O_3nano thin film structure wasfabricated on pattern vicinal substrate LAO (100) by photo-assisted MOCVD. Nucleationand growth processes of Y_2O_3nanostructure self-assembled as rows along the terraces ofpattern substrate were investigated with various growth parameters. It is found that densityand size of Y_2O_3nanostructures can be tuned and well controlled by varying substratetemperature (Ts) and oxygen partial pressure. With elevating Ts, the nanostructures graduallygrow larger and sparser. This phenomenon could be illustrated by two competitive kineticprocesses, i.e. surface diffusion of adatoms and yttrium desorption. Morphologies anddensity of these nanostructures were also influenced by variation of oxygen partial pressure.To further discuss the growth kinetics, a more clearly quasi-linear distribution was obtainedand the coarsening effect is modified by varying growth time. Solid cone shaped Y_2O_3nanostructures with relatively uniform size and density were prepared.
本论文采用光辅助MOCVD技术制备出了具有类单晶形貌，良好晶体结构，高临界电流密度的YBCO薄膜，J_c最高达到3.75MA/cm~2，详细分析了衬底生长温度，源挥发比例对薄膜形貌、结晶质量及超导性能的影响。以优化后的工艺条件为基础制备了高质量的YBCO厚膜，并研究了由于薄膜厚度增加所引起的薄膜性质的一些变化。
作为多层膜结构研究的前期准备工作，首次选用GdBCO作为以后研究多层膜结构的夹层材料。并首次采用光辅助MOCVD技术制备出了纯的GdBCO外延膜，研究了衬底温度、氧分压、组分等工艺条件对外延膜晶体质量、生长速率、超导性能的影响。系统的分析了不同厚度薄膜制备过程中薄膜的生长速率、微结构变化和应力释放现象，以及它们对薄膜的晶体质量和超导性质的影响。
选用了Y_2O_3纳米薄层结构作为另一种中间夹层材料。首次利于光辅助MOCVD技术在图形化衬底上进行了应力诱导Y_2O_3纳米薄层结构的自组装生长，并研究了制备过程中的热力学和成核动力学过程。利用高温热处理衬底产生的原子级晶格台阶实现了对Y_2O_3纳米结构在空间分布上的控制。从热力学的角度出发，研究了生长温度和氧分压对Y_2O_3纳米薄层结构生长的影响，并利用两种动力学过程的竞争机制对生长机理进行了分析。从生长动力学角度，研究了生长时间和退火处理时间对于Y_2O_3纳米结构生长的影响。
To improve the current carrying capacity of the superconducting film is an increasinglyurgent need for power applications of high-temperature superconductors. The value ofcritical current depends on the film thickness (d) and the critical current density (Jc). It iswell known that the critical current density of pure YBa_2Cu_3O_(7-δ)(YBCO) films can becomevery high due to a number of growth-induced structural defects such as dislocations. Forpractical applications, however, the flux pinning still needs to be further improved toovercome the vortex motion at high magnetic fields. Therefore, to obtain a larger currentcarrying capacity needs to seek a breakthrough in the thickness of the superconducting filmand the pinning centers. In this paper, photo-assisted metal organic chemical vapordeposition (MOCVD) epitaxial system was employed to fabricate REBCO high quality thickfilms and interlayers of multilayer structure, and their structure and properties wereinvestigated.
In this paper, high-quality YBCO epitaxial films were grown by a photo-assistedMOCVD technique, the films with single-crystal-like morphology, high crystalline andsuperconductive quality were characterized. The highest value of Jcis3.75MA cm~(-2)at77Kin self-field. The effects of substrate temperature and precursors’ proportion on morphology,crystallographic and superconductive quality were investigated. Base on the optimizedprocess conditions, high-quality YBCO thick films was fabricated by controlling thedeposition time. The reason why epitaxial YBCO thick films with high-qualitysingle-crystal-like morphology can be grown up to about2.1μm thick is illustrated from the point of view of photo activation. Meanwhile, the evaluation of film properties with variousthicknesses was systematically investigated. Therefore, the PhA-MOCVD technique mayprovide some advantages for high-rate growth of high-quality YBCO thick films over otherdeposition techniques for various important applications.
As the preliminary preparation for the research of multilayer structure, GdBa_2Cu_3O_7-δ(GdBCO) was firstly used as the interlayer. Photo-assisted MOCVD was employed tofabricate pure GdBCO films for the first time. The effects of substrate temperature (Ts) andoxygen partial pressure (PO2) on microstructure, growth rate and superconducting criticalcurrent density (Jc) were investigated. The (001) preferred orientation of the GdBCO filmswas enhanced with increasing Ts. Film growth rate and degree of texture were found to beinfluenced by PO2. The highly c-axis oriented GdBCO film with Jcof2.5MA/cm~2at77K inself-field was obtained at Tsof810°C and PO_2of4Torr, and the morphology of GdBCOfilm was characterized as single-crystal-like. A growth rate of0.107μm/min is realized bythe PhA-MOCVD technique.
High-quality GdBCO films with thicknesses of0.14-1.62μm were fabricated byPhA-MOCVD technique. Evaluation of film microstructure and strain-relaxationphenomenon in the growing films, and their effects on the crystallographic andsuperconducting properties of the GdBCO films were investigated. A dense and no grainboundary visible, single-crystal-like cross-sectional morphology was observed. For a0.31μm GdBCO film sample, the full width at half-maximum were0.08°and0.47°forout-of-plane and in-plane orientations, respectively. To our knowledge, this is the best valuereported to date for GdBCO heteroepitaxial films, which demonstrate that the films possesswell biaxial texture. The c-axis lattice parameters of the GdBCO films grown with differentthicknesses were used to determine the out-of-plane strain. The result shows that the straincould be gradually relieved as film thickness increasing. As films were getting thicker, theirJcvalues decrease gradually. This is mainly attributed to a lack of pinning centers in thethicker films.
We choose Y_2O_3nano thin film structure as another interlayer for the study of multilayer structure in future. Self-assembling of strain-induced Y_2O_3nano thin film structure wasfabricated on pattern vicinal substrate LAO (100) by photo-assisted MOCVD. Nucleationand growth processes of Y_2O_3nanostructure self-assembled as rows along the terraces ofpattern substrate were investigated with various growth parameters. It is found that densityand size of Y_2O_3nanostructures can be tuned and well controlled by varying substratetemperature (Ts) and oxygen partial pressure. With elevating Ts, the nanostructures graduallygrow larger and sparser. This phenomenon could be illustrated by two competitive kineticprocesses, i.e. surface diffusion of adatoms and yttrium desorption. Morphologies anddensity of these nanostructures were also influenced by variation of oxygen partial pressure.To further discuss the growth kinetics, a more clearly quasi-linear distribution was obtainedand the coarsening effect is modified by varying growth time. Solid cone shaped Y_2O_3nanostructures with relatively uniform size and density were prepared.
引文
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