实用化YBCO高温超导带材制备与性能研究
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摘要
YBCO高温超导带材具有临界电流密度高、不可逆场高以及交流损耗低等优点,在工业上具有广阔的应用前景,成为近年来超导技术发展的重点。针对YBCO高温超导带材实用化进程中存在的制备及性能方面的科学与技术问题,本文开展了以下四方面的系统性的研究工作：无磁性Cu-Ni合金基带制备及电化学抛光、CeO2/YSZ/Y2O3三层隔离层制备、YBCO超导层制备、YBCO超导带材力学性能。
一、无磁性Cu-Ni合金基带制备及电化学抛光研究
(1)在高变形量轧制,分级加热保温和高温退火工艺条件下,可获得高度立方织构的无磁性Cu-Ni合金基带。其中,轧制总加工率≥98%,道次平均轧制加工率≤10%,分级加热温度控制在300～400℃,退火温度控制在1000℃左右。
(2)研究发现,提高中合金的Ni含量、采用分级加热保温工艺以及严格控制高温退火温度和时间有利于Cu-Ni合金基带立方织构的形成和强化。对Cu-Ni合金基带立方织构的形成进行了理论解释。
(3)开展Cu-Ni合金电化学抛光工艺研究,Cu-Ni合金基带抛光后表面粗糙度小于9nm。研究了抛光液中甘油、添加剂的作用机理,探讨了电流密度和温度对抛光效果的影响。
二、十米CeO2/YSZ/Y2O3隔离层带材制备研究
(1)采用直流反应溅射法制备出高度立方织构的Y203种子层和CeO2/YSZ/Y2O3三层隔离层,隔离层表面均匀、平整、致密、无裂纹。系统研究了基带温度、溅射气压、H20分压和基带移动速度等工艺参数对隔离层生长的影响规律。
(2)采用直流反应溅射法制备出10米长CeO2/YSZ/Y2O3隔离层带材,带材具有均匀一致的立方织构,表面质量优良,具备生长高性能YBCO超导层的条件。
三、一米YBCO超导带材制备研究
(1)采用脉冲激光沉积法制备出1米长YBCO超导带材,YBCO超导层具有强立方织构,表面均匀、致密、无裂纹,厚度约为1.2μm,Tc=88K, ΔTc=1.3K,Jc达至1.5MA/cm2(77K,SF),Ic=50A (2mm宽样品),约合200A/cm。
(2)系统研究了基带温度、激光频率、退火时间和基带移动速度对YBCO薄膜质量的影响规律,研究了隔离层织构取向与YBCO超导层性能的关系。
四、YBCO超导带材力学性能研究
(1)采用基片曲率法和Stoney公式得出测算CeO2/YSZ/Y2O3隔离层残余应力的基本方法,深入研究了工作气压和衬底温度对隔离层残余应力的影响规律,总结了隔离层残余应力的形成机制。
(2)采用斜对称衍射和晶格常数法得出测算YBCO超导薄膜残余应力的基本方法,深入研究了YBCO超导薄膜厚度变化对其残余应力的影响规律,总结了YBCO超导薄膜残余应力的形成机制,并研究了残余应力对其超导性能的影响。
Due to its lower ac loses, better in-field performance, high critical current, and extensive applications in the industry, YBCO High-temperature superconductor (HTS) tapes have attracted the attention of the researchers worldwide. In order to resolve sicentific and technical problems in fabrication and properties of YBCO HTS tapes, four fields were systematically studied in this dissertation:Preparation and electropolishing of non-magnetic Cu-Ni alloy substrates, preparation of CeO2/YSZ/Y2O3buffer layer, preparation of YBCO layer, and mechanical properties of YBCO tapes.
1. Preparation and electropolishing of non-magnetic Cu-Ni alloy substrates
Highly cube textured non-magnetic Cu-Ni alloy substrates were prepared by heavy rolling (reduction more than98%) and high temperature annealing (1000℃) method. It is found that increasing Ni content of the alloy, grading heating, controlling annealing temperature and time would improve the cube texture of the Cu-Ni alloy. The dissertation also explained the forming process of cube texture of the Cu-Ni alloy substrates. Electropolishing process was studied and minimum roughness of less than9nm was got on Cu-Ni alloy substrates. The mechanism of glycerin and additive was discussed. The effect of critical current and temperature on the polishing was also invesgated.
2. Preparation of10-meter CeO2/YSZ/Y2O3buffer layer tape
Highly cube textured Y2O3seed layer and CeO2/YSZ/Y2O3buffer layer were fabricated by using DC reactive sputtering method. The buffer layers are smooth, dense and crac-free. The parameters of substrate temperature, total pressure, H2O pressure, and substrate moving speed were examined with respect to their role in the textureing process. A10-meter CeO2/YSZ/Y2O3buffer layer tape was obtained by using DC reactive sputtering method. The cube texture of the tape is uniform and surface of the tape is excellent.
3. Preparation of meter-long YBCO HTS tape
A meter-long YBCO HTS tape was fabricated by using PLD method. Transition temperature (Tc) of88K, critical current density (Jc) of1.5MA/cm2(77K,SF), and critical current (Ic) of50A (2mm wide) were obtained. The parameters of substrate temperature, laser pulse repetition rate, annealing time, and substrate moving speed were examined with respect to their role in the formation of YBCO layer.
4. Study of mechanical properties of YBCO tapes
Residual stress of CeO2/YSZ/Y2O3buffer layer was measured and calculated using Substrate Curvature Method and Stoney Formula. The effect of total pressure and substrate temperature on the residual stress was studied. A residual stress theoretical model of CeO2/YSZ/Y2O3buffer layer was put forward. On the other hand, residual stress of YBCO layer was measured and calculated using Skew Symmetric Diffraction and Lattice Parameter method. The effect of film thickness on the residual stress and the effect of stress on the properties were studied. A residual stress theoretical model of YBCO layer was put forward too.
一、无磁性Cu-Ni合金基带制备及电化学抛光研究
(1)在高变形量轧制,分级加热保温和高温退火工艺条件下,可获得高度立方织构的无磁性Cu-Ni合金基带。其中,轧制总加工率≥98%,道次平均轧制加工率≤10%,分级加热温度控制在300～400℃,退火温度控制在1000℃左右。
(2)研究发现,提高中合金的Ni含量、采用分级加热保温工艺以及严格控制高温退火温度和时间有利于Cu-Ni合金基带立方织构的形成和强化。对Cu-Ni合金基带立方织构的形成进行了理论解释。
(3)开展Cu-Ni合金电化学抛光工艺研究,Cu-Ni合金基带抛光后表面粗糙度小于9nm。研究了抛光液中甘油、添加剂的作用机理,探讨了电流密度和温度对抛光效果的影响。
二、十米CeO2/YSZ/Y2O3隔离层带材制备研究
(1)采用直流反应溅射法制备出高度立方织构的Y203种子层和CeO2/YSZ/Y2O3三层隔离层,隔离层表面均匀、平整、致密、无裂纹。系统研究了基带温度、溅射气压、H20分压和基带移动速度等工艺参数对隔离层生长的影响规律。
(2)采用直流反应溅射法制备出10米长CeO2/YSZ/Y2O3隔离层带材,带材具有均匀一致的立方织构,表面质量优良,具备生长高性能YBCO超导层的条件。
三、一米YBCO超导带材制备研究
(1)采用脉冲激光沉积法制备出1米长YBCO超导带材,YBCO超导层具有强立方织构,表面均匀、致密、无裂纹,厚度约为1.2μm,Tc=88K, ΔTc=1.3K,Jc达至1.5MA/cm2(77K,SF),Ic=50A (2mm宽样品),约合200A/cm。
(2)系统研究了基带温度、激光频率、退火时间和基带移动速度对YBCO薄膜质量的影响规律,研究了隔离层织构取向与YBCO超导层性能的关系。
四、YBCO超导带材力学性能研究
(1)采用基片曲率法和Stoney公式得出测算CeO2/YSZ/Y2O3隔离层残余应力的基本方法,深入研究了工作气压和衬底温度对隔离层残余应力的影响规律,总结了隔离层残余应力的形成机制。
(2)采用斜对称衍射和晶格常数法得出测算YBCO超导薄膜残余应力的基本方法,深入研究了YBCO超导薄膜厚度变化对其残余应力的影响规律,总结了YBCO超导薄膜残余应力的形成机制,并研究了残余应力对其超导性能的影响。
Due to its lower ac loses, better in-field performance, high critical current, and extensive applications in the industry, YBCO High-temperature superconductor (HTS) tapes have attracted the attention of the researchers worldwide. In order to resolve sicentific and technical problems in fabrication and properties of YBCO HTS tapes, four fields were systematically studied in this dissertation:Preparation and electropolishing of non-magnetic Cu-Ni alloy substrates, preparation of CeO2/YSZ/Y2O3buffer layer, preparation of YBCO layer, and mechanical properties of YBCO tapes.
1. Preparation and electropolishing of non-magnetic Cu-Ni alloy substrates
Highly cube textured non-magnetic Cu-Ni alloy substrates were prepared by heavy rolling (reduction more than98%) and high temperature annealing (1000℃) method. It is found that increasing Ni content of the alloy, grading heating, controlling annealing temperature and time would improve the cube texture of the Cu-Ni alloy. The dissertation also explained the forming process of cube texture of the Cu-Ni alloy substrates. Electropolishing process was studied and minimum roughness of less than9nm was got on Cu-Ni alloy substrates. The mechanism of glycerin and additive was discussed. The effect of critical current and temperature on the polishing was also invesgated.
2. Preparation of10-meter CeO2/YSZ/Y2O3buffer layer tape
Highly cube textured Y2O3seed layer and CeO2/YSZ/Y2O3buffer layer were fabricated by using DC reactive sputtering method. The buffer layers are smooth, dense and crac-free. The parameters of substrate temperature, total pressure, H2O pressure, and substrate moving speed were examined with respect to their role in the textureing process. A10-meter CeO2/YSZ/Y2O3buffer layer tape was obtained by using DC reactive sputtering method. The cube texture of the tape is uniform and surface of the tape is excellent.
3. Preparation of meter-long YBCO HTS tape
A meter-long YBCO HTS tape was fabricated by using PLD method. Transition temperature (Tc) of88K, critical current density (Jc) of1.5MA/cm2(77K,SF), and critical current (Ic) of50A (2mm wide) were obtained. The parameters of substrate temperature, laser pulse repetition rate, annealing time, and substrate moving speed were examined with respect to their role in the formation of YBCO layer.
4. Study of mechanical properties of YBCO tapes
Residual stress of CeO2/YSZ/Y2O3buffer layer was measured and calculated using Substrate Curvature Method and Stoney Formula. The effect of total pressure and substrate temperature on the residual stress was studied. A residual stress theoretical model of CeO2/YSZ/Y2O3buffer layer was put forward. On the other hand, residual stress of YBCO layer was measured and calculated using Skew Symmetric Diffraction and Lattice Parameter method. The effect of film thickness on the residual stress and the effect of stress on the properties were studied. A residual stress theoretical model of YBCO layer was put forward too.
引文
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