YBCO涂层导体长带与厚膜制备技术及钉扎机制研究
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摘要
YBa2Cu3O7-δ (YBCO)高温超导材料的不可逆场高,在高温高场中仍保持较高的临界电流密度,具有很好的应用前景。对YBCO涂层导体长带制备技术的研究,提高它的载流能力和高场性能是应用的需求。本文采用脉冲激光沉积(PLD)方法,以获得高性能的YBCO涂层导体长带为目的,研究在带有隔离层CeO2/YSZ/Y2O3/NiW的金属基带上,连续沉积YBCO膜的制备技术,进而研究涂层导体厚膜的制备和磁通钉扎机制。
自主设计研发了适合连续制备长带的动态真空镀膜装置,使其完全满足长带样品脉冲激光沉积YBCO的需求。
研究了适用于该装置的PLD技术制备YBCO带材的基本参数及它们的相关性,主要包括脉冲激光能量、背底氧压、沉积温度、靶基距等参数。采用分幅照相法,对激光诱导等离子体的形态进行了观测和分析；并根据沉积温度对YBCO膜的织构取向和超导性能的影响,确定了这些基本参数的最佳范围。
研究了连续移动沉积YBCO带材的技术,尝试通过增加YBCO超导膜的厚度来提高其临界电流(Ic)。为此提出了两条技术路线来增加YBCO膜的厚度：(1)改变脉冲激光重复频率：(2)改变基带移动的速率。结果表明,通过改变这两个参数可以增加YBCO膜的厚度,但其Ic却在增加到50A后,不再随膜厚度的增加而进一步提高。分析认为导致电流随膜厚度增加而趋于饱和这一结果的原因有以下几点：(1)随厚度增加,衬底表面生长温度降低,导致YBCO膜表面容易出现a轴取向颗粒；(2)在某一厚度开始出现微裂纹,并伴随有孔洞的存在；(3)由于生长条件的微变动导致YBCO膜的结构取向有偏差；(4)衬底的化学稳定性和温度控制不当导致YBCO与隔离层界面发生界面反应；(5)非超导相或缺陷的存在致使转变温度Tc的转变宽度宽,存在拖尾等不利现象；(6)靶材的表面沟槽直接影响等离子体羽辉的形态,进而影响YBCO的成分：(7)气压的变化、基带的微动、测温方式的不当等因素都会引起沉积温度的变化。因此在制备技术上做了多方面的改进,严格控制各沉积参数的稳定性。同时提出了反复沉积,分层控制的方法,使得YBCO随厚度的增加,膜表面的平整性、致密性得到大幅度改善,YBCO膜面内面外取向性也随之得到提高,实现了无裂纹、平整、高质量的YBCO薄膜生长。
采用分层工艺和最佳实验参数：氧压30Pa,相对沉积温度730℃,激光能量195mJ,基带移动速率0.1mm／s,脉冲激光重复频率10Hz,在CeO2/YSZ/Y2O3/NiW金属基带上,成功制备出一米长YBCO涂层导体。X射线衍射(XRD)θ-2θ扫描显示了YBCO膜呈单一c轴取向,并在长度方向上进行了多点测量,其YBCO(103)面XRDφ-扫描和(005)面ω-扫描半高宽的最好结果分别为6.87°和3.60°。分段测量了YBCO的超导转变温度,结果表明,长度方向上,Tc值在90.1-91.7K的范围内,转变宽度△T住0.4-0.7K的范围：分段测量的临界电流大于200A/cm-width。
首次提出了“间歇式”的沉积方式,成功制备了一系列不同厚度的YBCO膜和BaZrO3掺杂的YBCO膜。当YBCO(?)莫的厚度达到2.0微米时,膜表面致密、平整,其临界电流密度(Jc)仍保持在106A/cm3(77K,OT)量级。分析表明,YBCO(?)其随厚度的增加保持着良好的晶体结构,并伴随有应力存在。同时发现掺为(?)BaZrO3的样品存在阳离子缺陷,这些缺陷可能起磁通钉扎中心的作用。
进一步对掺杂的YBCO膜进行了磁场下性能的研究。结果表明,掺杂BaZrO3(?)样品无论在零场还是外加磁场下,YBCO(?)莫的Jc都高于未掺杂的YBCO(?)膜,在77K、0T的外场下,掺药(?)YBCOJc达到3.16×106A／cm2：在77K、IT外场一下,Jc达到6.21×105A／cm2,与未掺杂(?)YBCO膜相比,Jc提高了约2倍。掺杂YBCO(?)膜在77K、1.6T时对应最大钉扎力为7.1GN/m3;在65K、3.7T对应最大钉扎力为47GN／m3,在3-5T的磁场范围钉扎力均保持在45GN/m3。
首次对不同厚度的掺杂和米掺杂YBCO单磁通区钉扎类型进行了分析。研究表明,随温度变化钉扎类型也在发生变化,在低中温区以δl钉扎为主。随着温度的升高,应力钉扎逐渐增强,直至应力钉扎起主导作用。
High temperature superconducting material YBa2Cu3O7-x(YBCO) intrinsically has high critical current density at high magnetic field, which is suitable for electric power applications. The purpose of this thesis is to develop the fabrication processes of meter long coated conductor in order to the high critical current of YBCO. The YBCO was deposited on NiW metal tape with the CeO2/YSZ/Y2O3buffer layer by using pulsed laser deposition (PLD). Furthermore, YBCO thick film and flux pinning mechanism were studied.
A home designed reel-to-reel PLD system was set up for continuously depositing meter-long YBCO tape. Our focus was first on the study of the basic deposition process parameters of the YBCO tapes, such as pulsed laser energy, background oxygen pressure, deposition temperature, and target to substrate distance, and their dependence. The images of the laser plasma were analyzed by a frame photography method, and the texture orientation and superconducting properties of the YBCO films at different deposition temperatures were studied. The optimized ranges of these basic parameters were determined.
With the optimized deposition parameters established, we studied the technology for reel to reel deposition of YBCO tapes. In order to improve the critical current Ic, we tried to increase YBCO film thickness through two approaches, one is increasing the laser pulse repetition rate, and the other is changing the reel to reel tape speed. It was found that although the YBCO film thickness was increased, the critical current maxed at50A and did not change significantly with increasing thickness. The saturation of Ic with increasing YBCO film happened. The reasons were as follow. The substrate surface temperature decreased as the YBCO film thickness increased, resulting in the formation of a-axis grains, and appearance of micro cracks and holes above certain film thickness. Process parameters affected the superconducting properties of the YBCO tapes in various ways. Minute fluctuations in the growth conditions resulted in deviation of the texture of part of the YBCO film from the preferred c-axis orientation; chemical instability of the substrate and deposition temperature drifting caused interface reaction between the YBCO film and the buffer layer; non-superconducting phases and other defects widened the transition width of the critical temperature Tc of the YBCO films; target surface roughness directly affected the shape of the plasma plume, therefore resulting in changes in the composition of the YBCO films; changes in chamber pressure, small movements of the substrate, and the way of the temperature measured all had an impact the stability of the deposition temperature on the YBCO films. Based on these experimental results, we modified our deposition processes by applying more rigorous control on the above mentioned parameters. A new multi-coating process was developed using layer by layer deposition process, which improved the YBCO texture, and produced in crack free, smooth, high quality YBCO films.
Using the multi-coating process and optimized parameters of30Pa oxygen pressure,730℃relative deposition temperature,195mJ laser energy,0.1mm/s reel to reel tape speed,10Hz laser pulse repetition rate, meter long YBCO coated conductor on the buffered tape was successfully fabricated. XRD0-20scan showed a pure c-axis YBCO texture. The best results of YBCO (103) XRD φ-scan and (005) ω-scan values are6.87°and3.60°, respectively. The critical transition temperature of the YBCO tape were typically as90.1-91.7K with0.4-0.7K transition widths. The critical current was over200A/cm-width at77K and OT.
An intermitted deposition method was first proposed for fabricating YBCO thick films with and without BaZrO3doped. YBCO films with thicknesses up to2.0μm demonstrated critical current densities in the order of106A/cm2. Analysis showed these films maintained better crystalline. The doping of BaZrO; generated flux pinning centers with cation disorder.
Further comparison of the superconducting properties of the doped and undoped YBCO films under magnetic field showed that the BaZrO3doped samples always had a higher critical current density than that of the pure YBCO. The doped YBCO film had a critical current density Jc of3.16x106A/cm2at77K,OT and6.21×105A/cm2at1T which was about twice of those of the undoped samples. The pinning force in the doped YBCO films was7.1GN/m3at77K and1.6T, and47GN/m3at65K and3.7T. The pinning force stayed on the level of45GN/m3under higher magnetic field ranging from3T to5T.
We also analyzed the pinning type of single flux pinning in the doped and undoped YBCO samples. It has showed that the pinning type changes with temperature. At low and medium temperature, they are mostly of δl pinning. As the temperature increased the amount of stress pinning increased, and eventually took the majority.
自主设计研发了适合连续制备长带的动态真空镀膜装置,使其完全满足长带样品脉冲激光沉积YBCO的需求。
研究了适用于该装置的PLD技术制备YBCO带材的基本参数及它们的相关性,主要包括脉冲激光能量、背底氧压、沉积温度、靶基距等参数。采用分幅照相法,对激光诱导等离子体的形态进行了观测和分析；并根据沉积温度对YBCO膜的织构取向和超导性能的影响,确定了这些基本参数的最佳范围。
研究了连续移动沉积YBCO带材的技术,尝试通过增加YBCO超导膜的厚度来提高其临界电流(Ic)。为此提出了两条技术路线来增加YBCO膜的厚度：(1)改变脉冲激光重复频率：(2)改变基带移动的速率。结果表明,通过改变这两个参数可以增加YBCO膜的厚度,但其Ic却在增加到50A后,不再随膜厚度的增加而进一步提高。分析认为导致电流随膜厚度增加而趋于饱和这一结果的原因有以下几点：(1)随厚度增加,衬底表面生长温度降低,导致YBCO膜表面容易出现a轴取向颗粒；(2)在某一厚度开始出现微裂纹,并伴随有孔洞的存在；(3)由于生长条件的微变动导致YBCO膜的结构取向有偏差；(4)衬底的化学稳定性和温度控制不当导致YBCO与隔离层界面发生界面反应；(5)非超导相或缺陷的存在致使转变温度Tc的转变宽度宽,存在拖尾等不利现象；(6)靶材的表面沟槽直接影响等离子体羽辉的形态,进而影响YBCO的成分：(7)气压的变化、基带的微动、测温方式的不当等因素都会引起沉积温度的变化。因此在制备技术上做了多方面的改进,严格控制各沉积参数的稳定性。同时提出了反复沉积,分层控制的方法,使得YBCO随厚度的增加,膜表面的平整性、致密性得到大幅度改善,YBCO膜面内面外取向性也随之得到提高,实现了无裂纹、平整、高质量的YBCO薄膜生长。
采用分层工艺和最佳实验参数：氧压30Pa,相对沉积温度730℃,激光能量195mJ,基带移动速率0.1mm／s,脉冲激光重复频率10Hz,在CeO2/YSZ/Y2O3/NiW金属基带上,成功制备出一米长YBCO涂层导体。X射线衍射(XRD)θ-2θ扫描显示了YBCO膜呈单一c轴取向,并在长度方向上进行了多点测量,其YBCO(103)面XRDφ-扫描和(005)面ω-扫描半高宽的最好结果分别为6.87°和3.60°。分段测量了YBCO的超导转变温度,结果表明,长度方向上,Tc值在90.1-91.7K的范围内,转变宽度△T住0.4-0.7K的范围：分段测量的临界电流大于200A/cm-width。
首次提出了“间歇式”的沉积方式,成功制备了一系列不同厚度的YBCO膜和BaZrO3掺杂的YBCO膜。当YBCO(?)莫的厚度达到2.0微米时,膜表面致密、平整,其临界电流密度(Jc)仍保持在106A/cm3(77K,OT)量级。分析表明,YBCO(?)其随厚度的增加保持着良好的晶体结构,并伴随有应力存在。同时发现掺为(?)BaZrO3的样品存在阳离子缺陷,这些缺陷可能起磁通钉扎中心的作用。
进一步对掺杂的YBCO膜进行了磁场下性能的研究。结果表明,掺杂BaZrO3(?)样品无论在零场还是外加磁场下,YBCO(?)莫的Jc都高于未掺杂的YBCO(?)膜,在77K、0T的外场下,掺药(?)YBCOJc达到3.16×106A／cm2：在77K、IT外场一下,Jc达到6.21×105A／cm2,与未掺杂(?)YBCO膜相比,Jc提高了约2倍。掺杂YBCO(?)膜在77K、1.6T时对应最大钉扎力为7.1GN/m3;在65K、3.7T对应最大钉扎力为47GN／m3,在3-5T的磁场范围钉扎力均保持在45GN/m3。
首次对不同厚度的掺杂和米掺杂YBCO单磁通区钉扎类型进行了分析。研究表明,随温度变化钉扎类型也在发生变化,在低中温区以δl钉扎为主。随着温度的升高,应力钉扎逐渐增强,直至应力钉扎起主导作用。
High temperature superconducting material YBa2Cu3O7-x(YBCO) intrinsically has high critical current density at high magnetic field, which is suitable for electric power applications. The purpose of this thesis is to develop the fabrication processes of meter long coated conductor in order to the high critical current of YBCO. The YBCO was deposited on NiW metal tape with the CeO2/YSZ/Y2O3buffer layer by using pulsed laser deposition (PLD). Furthermore, YBCO thick film and flux pinning mechanism were studied.
A home designed reel-to-reel PLD system was set up for continuously depositing meter-long YBCO tape. Our focus was first on the study of the basic deposition process parameters of the YBCO tapes, such as pulsed laser energy, background oxygen pressure, deposition temperature, and target to substrate distance, and their dependence. The images of the laser plasma were analyzed by a frame photography method, and the texture orientation and superconducting properties of the YBCO films at different deposition temperatures were studied. The optimized ranges of these basic parameters were determined.
With the optimized deposition parameters established, we studied the technology for reel to reel deposition of YBCO tapes. In order to improve the critical current Ic, we tried to increase YBCO film thickness through two approaches, one is increasing the laser pulse repetition rate, and the other is changing the reel to reel tape speed. It was found that although the YBCO film thickness was increased, the critical current maxed at50A and did not change significantly with increasing thickness. The saturation of Ic with increasing YBCO film happened. The reasons were as follow. The substrate surface temperature decreased as the YBCO film thickness increased, resulting in the formation of a-axis grains, and appearance of micro cracks and holes above certain film thickness. Process parameters affected the superconducting properties of the YBCO tapes in various ways. Minute fluctuations in the growth conditions resulted in deviation of the texture of part of the YBCO film from the preferred c-axis orientation; chemical instability of the substrate and deposition temperature drifting caused interface reaction between the YBCO film and the buffer layer; non-superconducting phases and other defects widened the transition width of the critical temperature Tc of the YBCO films; target surface roughness directly affected the shape of the plasma plume, therefore resulting in changes in the composition of the YBCO films; changes in chamber pressure, small movements of the substrate, and the way of the temperature measured all had an impact the stability of the deposition temperature on the YBCO films. Based on these experimental results, we modified our deposition processes by applying more rigorous control on the above mentioned parameters. A new multi-coating process was developed using layer by layer deposition process, which improved the YBCO texture, and produced in crack free, smooth, high quality YBCO films.
Using the multi-coating process and optimized parameters of30Pa oxygen pressure,730℃relative deposition temperature,195mJ laser energy,0.1mm/s reel to reel tape speed,10Hz laser pulse repetition rate, meter long YBCO coated conductor on the buffered tape was successfully fabricated. XRD0-20scan showed a pure c-axis YBCO texture. The best results of YBCO (103) XRD φ-scan and (005) ω-scan values are6.87°and3.60°, respectively. The critical transition temperature of the YBCO tape were typically as90.1-91.7K with0.4-0.7K transition widths. The critical current was over200A/cm-width at77K and OT.
An intermitted deposition method was first proposed for fabricating YBCO thick films with and without BaZrO3doped. YBCO films with thicknesses up to2.0μm demonstrated critical current densities in the order of106A/cm2. Analysis showed these films maintained better crystalline. The doping of BaZrO; generated flux pinning centers with cation disorder.
Further comparison of the superconducting properties of the doped and undoped YBCO films under magnetic field showed that the BaZrO3doped samples always had a higher critical current density than that of the pure YBCO. The doped YBCO film had a critical current density Jc of3.16x106A/cm2at77K,OT and6.21×105A/cm2at1T which was about twice of those of the undoped samples. The pinning force in the doped YBCO films was7.1GN/m3at77K and1.6T, and47GN/m3at65K and3.7T. The pinning force stayed on the level of45GN/m3under higher magnetic field ranging from3T to5T.
We also analyzed the pinning type of single flux pinning in the doped and undoped YBCO samples. It has showed that the pinning type changes with temperature. At low and medium temperature, they are mostly of δl pinning. As the temperature increased the amount of stress pinning increased, and eventually took the majority.
引文
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