高分子輔助化學(xué)溶液沉積法制備涂層導(dǎo)體緩沖層和超導(dǎo)層
發(fā)布時(shí)間：2019-01-19 08:38
【摘要】：涂層導(dǎo)體的制備技術(shù)和大規(guī)模工業(yè)應(yīng)用是當(dāng)前超導(dǎo)材料研究的熱點(diǎn)。本論文基于涂層導(dǎo)體實(shí)用化進(jìn)程中的織構(gòu)優(yōu)良,致密度高,載流能力強(qiáng)的要求,以涂層導(dǎo)體緩沖層和超導(dǎo)層的化學(xué)制備技術(shù)為研究對(duì)象,開(kāi)發(fā)出了一系列低成本、高效率的制備高性能涂層導(dǎo)體的技術(shù)。通過(guò)對(duì)具有自主知識(shí)產(chǎn)權(quán)的REBiO3緩沖層材料的RE位進(jìn)行摻雜獲得了一系列新型的緩沖層材料,并得到了表面具有不同形狀的納米顆粒析出相的Sm0.5Ca0.5BiO3和Eu0.6Sr0.4BiO3緩沖層材料,取得了一些有意義的結(jié)果。 論文第1章闡述了涂層導(dǎo)體研究開(kāi)發(fā)的科學(xué)意義和實(shí)用價(jià)值,重點(diǎn)歸納與介紹了當(dāng)前主流的緩沖層材料與制備技術(shù)。 第2章系統(tǒng)地闡述了第二代高溫超導(dǎo)帶材(即涂層導(dǎo)體)的基本實(shí)驗(yàn)原理與方法。重點(diǎn)介紹了化學(xué)溶液沉積技術(shù)和外延生長(zhǎng)機(jī)理。對(duì)該技術(shù)的分類(lèi)、前驅(qū)物、制膠的工藝流程等進(jìn)行了闡述。 第3章對(duì)本論文涉及的實(shí)驗(yàn)方法和表征手段進(jìn)行了闡述。實(shí)驗(yàn)方法方面,介紹了高分子輔助化學(xué)溶液沉積(PA-CSD)法制備涂層導(dǎo)體緩沖層與超導(dǎo)層的一般流程與相關(guān)技術(shù)參數(shù)。表征手段方面,對(duì)本論文涉及的相結(jié)構(gòu)、微結(jié)構(gòu)、電磁性能表征的手段進(jìn)行了介紹。 第4章重點(diǎn)介紹了SmBiO3緩沖層在單晶基底LaA1O3以及在NiO緩沖層上的PA-CSD法的制備技術(shù)。并且初步成功地完成了NiW/NiO (SOE)/SmBiO3(PA-CSD)/YBCO(PA-CSD)這種新穎與低成本的涂層導(dǎo)體結(jié)構(gòu)的制備工作。隨后介紹了一系列PA-CSD法制備傳統(tǒng)緩沖層BaZrO3、SrZrO3、La2Zr207、以及導(dǎo)電緩沖層La0.7Sr0.3MnO3的技術(shù),研究了各自的最佳熱處理工藝路線。結(jié)合高分子添加劑的化學(xué)性質(zhì)和熱力學(xué)特性提出了一種解釋單次涂敷臨界厚度提高的機(jī)制。結(jié)果表明,高分子輔助沉積制備技術(shù)是一種成本低廉、易于推廣的緩沖層制備技術(shù)。最后,在REBiO3緩沖層基礎(chǔ)上,介紹了REBiO3中的RE位用Ca或Pb替代的研究工作。并據(jù)此在LaA1O3(100)單晶基底上制得織構(gòu)良好、表面平整致密的Sm1-xCaxBiO3Eu1-xCaxBiO3、Gd1-xCaxBiO3、Gd1-xPbxBiO3外延薄膜,這為調(diào)節(jié)REBiO3的晶格和導(dǎo)電性提供了新的途徑,并得到了一系列新型的緩沖層材料。此外,在本章中特別介紹了緩沖層材料Sm0.5Ca0.5BiO3和Eu0.6Sr0.4BiO3.在其表面可以制備出納米級(jí)的不同形狀的析出相,進(jìn)而可能作為釘扎中心來(lái)研究其對(duì)YBCO涂層導(dǎo)體在磁場(chǎng)下的臨界電流密度的影響。 第5章討論了EuBa2Cu3O7-x (EuBCO)薄膜在單晶基底LaA1O3(100)上的PA-CSD法的制備技術(shù)。利用自主開(kāi)發(fā)的基于金屬乙酸鹽的高分子輔助無(wú)氟化學(xué)溶液沉積技術(shù),在氮?dú)鈿夥罩蠰aAIOa (100)單晶基底上生長(zhǎng)了EuBCO薄膜。通過(guò)對(duì)熱處理過(guò)程進(jìn)行優(yōu)化,制得了厚度為290nm、雙軸織構(gòu)良好、表面致密平整和無(wú)微裂紋的EuBCO薄膜,且臨界超導(dǎo)轉(zhuǎn)變溫度為91K,77K自場(chǎng)下的臨界電流密度約為2.4MA/cm2。最后,對(duì)用PA-CSD法的制備超導(dǎo)薄膜的面內(nèi)面外取向生長(zhǎng)機(jī)理作了詳細(xì)的討論與解釋。
[Abstract]:The preparation technology and large-scale industrial application of coated conductors are the hot spots in the research of superconducting materials. Based on the requirements of good texture, high density and high current carrying capacity in the practical process of coating conductor, a series of low cost have been developed based on the chemical preparation technology of coating conductor buffer layer and superconducting layer. Efficient preparation of high performance coated conductors. A series of novel buffer layer materials were obtained by doping RE sites of REBiO3 buffer layer materials with independent intellectual property rights. Sm0.5Ca0.5BiO3 and Eu0.6Sr0.4BiO3 buffer layer materials with different shapes of precipitates were obtained, and some significant results were obtained. In chapter 1, the scientific significance and practical value of the research and development of coated conductors are described, and the current mainstream buffer layer materials and preparation techniques are summarized and introduced emphatically. In chapter 2, the basic experimental principle and method of the second generation high temperature superconducting tape (i.e. coated conductor) are systematically described. The chemical solution deposition technology and epitaxial growth mechanism are introduced in detail. The classification, precursor and technological process of this technology are described. Chapter 3 describes the experimental methods and characterization methods involved in this paper. In terms of experimental methods, the general process and related technical parameters of polymer assisted chemical solution deposition (PA-CSD) for preparation of buffer layer and superconducting layer of coating conductor are introduced. In the aspect of characterization, the phase structure, microstructure and electromagnetic properties of this paper are introduced. In chapter 4, the preparation technology of SmBiO3 buffer layer on single crystal substrate LaA1O3 and on NiO buffer layer by PA-CSD method is introduced. NiW/NiO (SOE) / SmBiO3 (PA-CSD) / YBCO (PA-CSD), a novel and low cost coated conductor structure, has been successfully prepared. Then a series of techniques of preparing traditional buffer layer BaZrO3,SrZrO3,La2Zr207, and conductive buffer layer La0.7Sr0.3MnO3 by PA-CSD method are introduced and their optimal heat treatment processes are studied. Based on the chemical and thermodynamic properties of polymer additives, a mechanism is proposed to explain the increase of critical thickness of single coating. The results show that polymer assisted deposition is a low cost and easy to be popularized buffer layer preparation technology. Finally, on the basis of REBiO3 buffer layer, the research work of replacing RE bits with Ca or Pb in REBiO3 is introduced. On the basis of this, Sm1-xCaxBiO3Eu1-xCaxBiO3,Gd1-xPbxBiO3 epitaxial films with good texture and smooth and compact surface were prepared on LaA1O3 (100) single crystal substrates, which provided a new way to regulate the lattice and conductivity of REBiO3. A series of new buffer layer materials were obtained. In addition, in this chapter, the buffer layer materials Sm0.5Ca0.5BiO3 and Eu0.6Sr0.4BiO3. are introduced in particular. Nanoscale precipitates with different shapes can be prepared on the surface, which may serve as pinning centers to study the effect of nanoscale precipitates on the critical current density of YBCO coating conductors in magnetic field. In chapter 5, the preparation technology of EuBa2Cu3O7-x (EuBCO) thin films on LaA1O3 (100) single crystal substrate by PA-CSD method is discussed. EuBCO thin films were grown on LaAIOa (100) single crystal substrates in nitrogen atmosphere by polymeric polymer assisted fluorine-free chemical solution deposition based on metal acetate. By optimizing the heat treatment process, the EuBCO thin films with a thickness of 290 nm, good biaxial texture, compact and flat surface and no microcracks have been prepared. The critical current density of the superconducting films is about 2.4 Ma / cm ~ (2) at 91K ~ (77) K self-field. Finally, the in-plane and out-of-plane orientation growth mechanism of superconducting thin films prepared by PA-CSD method is discussed and explained in detail.
【學(xué)位授予單位】：西南交通大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2013
【分類(lèi)號(hào)】：TB306
本文編號(hào)：2411193
[Abstract]:The preparation technology and large-scale industrial application of coated conductors are the hot spots in the research of superconducting materials. Based on the requirements of good texture, high density and high current carrying capacity in the practical process of coating conductor, a series of low cost have been developed based on the chemical preparation technology of coating conductor buffer layer and superconducting layer. Efficient preparation of high performance coated conductors. A series of novel buffer layer materials were obtained by doping RE sites of REBiO3 buffer layer materials with independent intellectual property rights. Sm0.5Ca0.5BiO3 and Eu0.6Sr0.4BiO3 buffer layer materials with different shapes of precipitates were obtained, and some significant results were obtained. In chapter 1, the scientific significance and practical value of the research and development of coated conductors are described, and the current mainstream buffer layer materials and preparation techniques are summarized and introduced emphatically. In chapter 2, the basic experimental principle and method of the second generation high temperature superconducting tape (i.e. coated conductor) are systematically described. The chemical solution deposition technology and epitaxial growth mechanism are introduced in detail. The classification, precursor and technological process of this technology are described. Chapter 3 describes the experimental methods and characterization methods involved in this paper. In terms of experimental methods, the general process and related technical parameters of polymer assisted chemical solution deposition (PA-CSD) for preparation of buffer layer and superconducting layer of coating conductor are introduced. In the aspect of characterization, the phase structure, microstructure and electromagnetic properties of this paper are introduced. In chapter 4, the preparation technology of SmBiO3 buffer layer on single crystal substrate LaA1O3 and on NiO buffer layer by PA-CSD method is introduced. NiW/NiO (SOE) / SmBiO3 (PA-CSD) / YBCO (PA-CSD), a novel and low cost coated conductor structure, has been successfully prepared. Then a series of techniques of preparing traditional buffer layer BaZrO3,SrZrO3,La2Zr207, and conductive buffer layer La0.7Sr0.3MnO3 by PA-CSD method are introduced and their optimal heat treatment processes are studied. Based on the chemical and thermodynamic properties of polymer additives, a mechanism is proposed to explain the increase of critical thickness of single coating. The results show that polymer assisted deposition is a low cost and easy to be popularized buffer layer preparation technology. Finally, on the basis of REBiO3 buffer layer, the research work of replacing RE bits with Ca or Pb in REBiO3 is introduced. On the basis of this, Sm1-xCaxBiO3Eu1-xCaxBiO3,Gd1-xPbxBiO3 epitaxial films with good texture and smooth and compact surface were prepared on LaA1O3 (100) single crystal substrates, which provided a new way to regulate the lattice and conductivity of REBiO3. A series of new buffer layer materials were obtained. In addition, in this chapter, the buffer layer materials Sm0.5Ca0.5BiO3 and Eu0.6Sr0.4BiO3. are introduced in particular. Nanoscale precipitates with different shapes can be prepared on the surface, which may serve as pinning centers to study the effect of nanoscale precipitates on the critical current density of YBCO coating conductors in magnetic field. In chapter 5, the preparation technology of EuBa2Cu3O7-x (EuBCO) thin films on LaA1O3 (100) single crystal substrate by PA-CSD method is discussed. EuBCO thin films were grown on LaAIOa (100) single crystal substrates in nitrogen atmosphere by polymeric polymer assisted fluorine-free chemical solution deposition based on metal acetate. By optimizing the heat treatment process, the EuBCO thin films with a thickness of 290 nm, good biaxial texture, compact and flat surface and no microcracks have been prepared. The critical current density of the superconducting films is about 2.4 Ma / cm ~ (2) at 91K ~ (77) K self-field. Finally, the in-plane and out-of-plane orientation growth mechanism of superconducting thin films prepared by PA-CSD method is discussed and explained in detail.
【學(xué)位授予單位】：西南交通大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2013
【分類(lèi)號(hào)】：TB306
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