采用光辅助MOCVD方法生长YBCO薄膜和厚膜及其特性研究
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摘要
YBa2Cu3O7-δ(YBCO)材料在弱电方面的应用,特别是微波通讯所需的微波滤波器方面已经走上了实用化的道路。但是,制作高温超导滤波器所需的核心部分原材料,高质量双面YBCO高温超导体薄膜在国内仍然很难大批量提供。因此,为了解决这一难题,我们利用自行设计和搭建的光辅助MOCVD(photo-assisted Metel-organic Chemical Vapor Deposition)系统制备了高质量YBCO薄膜,并对其性能做了较为系统的研究。
通过我们自行搭建的光辅助MOCVD系统,不断优化长膜实验条件,包括衬底温度、三种金属有机源的挥发温度、载气及氧气和一氧化二氮的流量、生长时间、及生长总压等,制备出了质量比较高的YBCO高温超导膜。
在优化制膜实验过程中,首次通过计算机模拟了第一台石英反应室内部气流、压力、温度等参数的分布情况。通过与实验结果对比,发现模拟与实验基本吻合,数学上的模拟对于反应室结构的设计非常有参考意义。
同时进一步分析了金属有机源的热学特性,分析了金属有机源对薄膜表面的影响,通过改进源炉内部的内罐结构,改善了源挥发的均匀性。
通过计算机编程控制三种金属有机源挥发过程的温度,使得三种源可以在相对较长的时间内(15分钟)实现按预定比例均匀供给,薄膜的厚度可以达到4.5μm。对YBCO外延膜的厚度可以进行有效的控制,生长小面积(3×10cm)YBCO薄膜及厚膜(膜厚在1μm以上者)的重复率已经达到了80%以上。这一改进对实现高温超导膜产业化生产的目标具有重要意义。
本论文主要目的是为以光辅助MOCVD法制备大面积高质量YBCO外延膜作前期必需的准备工作,例如膜生长参数的优化及有效控制膜的厚度。
Many HTS superconductors are being engineered for use in high-current applications. In these HTS superconductors, because of its excellent electrical property high temperature superconductor (high-Tc) YBa2Cu3O7-x (YBCO) thin films have significant potential for applications in microwave devices, so more and more people attach importance to it. For these reason we plan to applied high quality YBCO thin films on larger area LAO(100) substrates by photo-assisted MOCVD. We have designed and assembled two photo-assisted MOCVD systems, one of them has a quartz reactor, the other one has a reactor made of stainless steel. In this study a systemic study of the characteristic of YBCO films prepared by the first photo-assisted MOCVD systems whose reactor was made of quartz was described.
1. Design of the photo-assisted MOCVD systems
Two photo-assisted MOCVD systems were designed and assembled. The precursors(Y(tmhd)、Ba(tmhd) and Cu(tmhd) ) used in our MOCVD system are solid state under room temperature, moreover they can not boil away easily under more higher temperature. So in our MOCVD systems the pipelines should be more shorter and can not have many turnings. The system is made up of eight parts, they are gas purifying plants, gas transport plants, precursor -supply system, gas mixing plants, lamp house, the reactor, 3 2 2 temperature control device and tail gas treatment. As yet these two photo-assisted MOCVD systems are running well. After the MOCVD system was fit in we optimized the MOCVD system with a quartz reactor.
2. Enactment of the gas flows, substrate temperature and the chamber pressure
We find the optimal parameters for YBCO thin films prepared by the photo-assisted MOCVD system: The substrate temperature is between 825℃and 855℃, the carrier gas flows of the Ba(tmhd)2,Y(tmhd)3,Cu(tmhd)2 are 300-450 sccm,100-150 sccm and 100-150 sccm, respectively;the O2 and N2O flow are 300-450 sccm and 200-300 sccm, respectively;the operating pressure is between 6 torr and 8 torr.
3. Hot wall and cold wall
We compared the characteristic of the YBCO films that prepared by hot wall and cold wall MOCVD, and find that the purely c-axis YBCO can prepared by cold wall MOCVD more easily.
4. The predominance of processing electronic materials by photo
We analyzed the predominance of processing electronic materials by photo relative to that by heat. We know that chemical or physical reaction thermal dissociation is fundamentally limited by Boltzmann distribution or thermal activation, but light in the UV, visible, as well as IR region can supply the necessary thermal energy to the sample. Various film preparation techniques, such as laser ablation, magnetron sputtering, and metal-organic chemical vapor deposition (MOCVD), have been utilized for epitaxial growth of high quality YBCO films. Among them, photo-assisted MOCVD technique has its two obvious advantages, the capability to grow both thin and thick high-quality YBCO films, one is YBCO films can be prepared with very high growth rate(above 200nm/min) another is YBCO films grown by photo-assisted MOCVD have single-crystal-like qualities, no SEM visualizable grain boundaries. So this technique has the capability to grow both thin and thick high-quality YBCO films with high growth rate. All of these advantages are all because of the photo assisting. In the photo-assisted MOCVD system, if the temperature of the substrate is settled, when the height of the substrate is changed the power of the lamps will change. And the color temperature of the filament will change according to the power. We know that in black-body radiation when the temperature of the blackbody is increased the energy eradiated will increase, so the wavelengh of the light that eradiated from blackbody is shorter. So in the experimental we set the power of the lemps beyound 85% when YBCO growing, here the color temperature of the filament is higher than 3000K the light that eradiated from filament include UV, visible, as well as IR region.
5. Chamber pressure and characteristic of the YBCO films
We analyzed how the chamber pressure effect on the characteristic of the YBCO films. The crystal structures of YBCO films grown under different chamber pressure were analyzed by the assist of SEM and XRD-2θscan. In our system if growth temperature is fixed, as the chamber pressure increasing the growth of pure c-axis YBCO films will change to growth of a-axis YBCO films, and the growth rate will increase at the begining and then decrease. From these experiences we find the optimization of the chamber pressure for pure c-axis YBCO grown.
6. Simulation for gas flow patterns and temperature
A three-dimensional simulation for gas flow patterns was conducted with commercial software FLUENT 6.0 for the first time. In the simulation, growth temperature, chamber pressure and growth time were all fixed; the only process variable was the susceptor inclination angle. The temperature of the substrate change tinily when this angle is changed. But as the angle changes, the gas flow pattern in the reactor chamber is changed accordingly. This change of gas flow pattern affect the growth mechanism of the growing YBCO films. And the experimental results were found to be well correlated with the simulations. We find that the simulation is very useful for the experimental. The experimental and the simulation show all show that when the angle between the axis of gas inlet and the susceptor surface is 22.5o the YBCO films have best characteristic.
7. The barium precursor’s sublimation/evaporation can not be well controlled and the solution
From the experimental we find that the barium precursor’s sublimation/evaporation can not be well controlled. We solved this problem by mending the structure of the precursors’ovens.
8. The thickness of the YBCO films can be controled
By evaporating the barium precursor employed with its heating temperature being appropriately programmed during the time interval of film growth the steady time of the barium precursor’s evaporating can last 15 minutes. By this method the thickness of the YBCO films can be well controlled under 4.5μm. And the characteristic of the YBCO thick films is as well as that of the thin films. The XRD-ωscan of two YBCO films (0.6μm and 4.5μm) with different thickness were analyzed, the FWHM are 0.29o and 0.30o.
通过我们自行搭建的光辅助MOCVD系统,不断优化长膜实验条件,包括衬底温度、三种金属有机源的挥发温度、载气及氧气和一氧化二氮的流量、生长时间、及生长总压等,制备出了质量比较高的YBCO高温超导膜。
在优化制膜实验过程中,首次通过计算机模拟了第一台石英反应室内部气流、压力、温度等参数的分布情况。通过与实验结果对比,发现模拟与实验基本吻合,数学上的模拟对于反应室结构的设计非常有参考意义。
同时进一步分析了金属有机源的热学特性,分析了金属有机源对薄膜表面的影响,通过改进源炉内部的内罐结构,改善了源挥发的均匀性。
通过计算机编程控制三种金属有机源挥发过程的温度,使得三种源可以在相对较长的时间内(15分钟)实现按预定比例均匀供给,薄膜的厚度可以达到4.5μm。对YBCO外延膜的厚度可以进行有效的控制,生长小面积(3×10cm)YBCO薄膜及厚膜(膜厚在1μm以上者)的重复率已经达到了80%以上。这一改进对实现高温超导膜产业化生产的目标具有重要意义。
本论文主要目的是为以光辅助MOCVD法制备大面积高质量YBCO外延膜作前期必需的准备工作,例如膜生长参数的优化及有效控制膜的厚度。
Many HTS superconductors are being engineered for use in high-current applications. In these HTS superconductors, because of its excellent electrical property high temperature superconductor (high-Tc) YBa2Cu3O7-x (YBCO) thin films have significant potential for applications in microwave devices, so more and more people attach importance to it. For these reason we plan to applied high quality YBCO thin films on larger area LAO(100) substrates by photo-assisted MOCVD. We have designed and assembled two photo-assisted MOCVD systems, one of them has a quartz reactor, the other one has a reactor made of stainless steel. In this study a systemic study of the characteristic of YBCO films prepared by the first photo-assisted MOCVD systems whose reactor was made of quartz was described.
1. Design of the photo-assisted MOCVD systems
Two photo-assisted MOCVD systems were designed and assembled. The precursors(Y(tmhd)、Ba(tmhd) and Cu(tmhd) ) used in our MOCVD system are solid state under room temperature, moreover they can not boil away easily under more higher temperature. So in our MOCVD systems the pipelines should be more shorter and can not have many turnings. The system is made up of eight parts, they are gas purifying plants, gas transport plants, precursor -supply system, gas mixing plants, lamp house, the reactor, 3 2 2 temperature control device and tail gas treatment. As yet these two photo-assisted MOCVD systems are running well. After the MOCVD system was fit in we optimized the MOCVD system with a quartz reactor.
2. Enactment of the gas flows, substrate temperature and the chamber pressure
We find the optimal parameters for YBCO thin films prepared by the photo-assisted MOCVD system: The substrate temperature is between 825℃and 855℃, the carrier gas flows of the Ba(tmhd)2,Y(tmhd)3,Cu(tmhd)2 are 300-450 sccm,100-150 sccm and 100-150 sccm, respectively;the O2 and N2O flow are 300-450 sccm and 200-300 sccm, respectively;the operating pressure is between 6 torr and 8 torr.
3. Hot wall and cold wall
We compared the characteristic of the YBCO films that prepared by hot wall and cold wall MOCVD, and find that the purely c-axis YBCO can prepared by cold wall MOCVD more easily.
4. The predominance of processing electronic materials by photo
We analyzed the predominance of processing electronic materials by photo relative to that by heat. We know that chemical or physical reaction thermal dissociation is fundamentally limited by Boltzmann distribution or thermal activation, but light in the UV, visible, as well as IR region can supply the necessary thermal energy to the sample. Various film preparation techniques, such as laser ablation, magnetron sputtering, and metal-organic chemical vapor deposition (MOCVD), have been utilized for epitaxial growth of high quality YBCO films. Among them, photo-assisted MOCVD technique has its two obvious advantages, the capability to grow both thin and thick high-quality YBCO films, one is YBCO films can be prepared with very high growth rate(above 200nm/min) another is YBCO films grown by photo-assisted MOCVD have single-crystal-like qualities, no SEM visualizable grain boundaries. So this technique has the capability to grow both thin and thick high-quality YBCO films with high growth rate. All of these advantages are all because of the photo assisting. In the photo-assisted MOCVD system, if the temperature of the substrate is settled, when the height of the substrate is changed the power of the lamps will change. And the color temperature of the filament will change according to the power. We know that in black-body radiation when the temperature of the blackbody is increased the energy eradiated will increase, so the wavelengh of the light that eradiated from blackbody is shorter. So in the experimental we set the power of the lemps beyound 85% when YBCO growing, here the color temperature of the filament is higher than 3000K the light that eradiated from filament include UV, visible, as well as IR region.
5. Chamber pressure and characteristic of the YBCO films
We analyzed how the chamber pressure effect on the characteristic of the YBCO films. The crystal structures of YBCO films grown under different chamber pressure were analyzed by the assist of SEM and XRD-2θscan. In our system if growth temperature is fixed, as the chamber pressure increasing the growth of pure c-axis YBCO films will change to growth of a-axis YBCO films, and the growth rate will increase at the begining and then decrease. From these experiences we find the optimization of the chamber pressure for pure c-axis YBCO grown.
6. Simulation for gas flow patterns and temperature
A three-dimensional simulation for gas flow patterns was conducted with commercial software FLUENT 6.0 for the first time. In the simulation, growth temperature, chamber pressure and growth time were all fixed; the only process variable was the susceptor inclination angle. The temperature of the substrate change tinily when this angle is changed. But as the angle changes, the gas flow pattern in the reactor chamber is changed accordingly. This change of gas flow pattern affect the growth mechanism of the growing YBCO films. And the experimental results were found to be well correlated with the simulations. We find that the simulation is very useful for the experimental. The experimental and the simulation show all show that when the angle between the axis of gas inlet and the susceptor surface is 22.5o the YBCO films have best characteristic.
7. The barium precursor’s sublimation/evaporation can not be well controlled and the solution
From the experimental we find that the barium precursor’s sublimation/evaporation can not be well controlled. We solved this problem by mending the structure of the precursors’ovens.
8. The thickness of the YBCO films can be controled
By evaporating the barium precursor employed with its heating temperature being appropriately programmed during the time interval of film growth the steady time of the barium precursor’s evaporating can last 15 minutes. By this method the thickness of the YBCO films can be well controlled under 4.5μm. And the characteristic of the YBCO thick films is as well as that of the thin films. The XRD-ωscan of two YBCO films (0.6μm and 4.5μm) with different thickness were analyzed, the FWHM are 0.29o and 0.30o.
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