NdBCO厚膜籽晶生长YBCO块体材料

本研究采用液相外延生长(Liquid phase epitaxy,简称LPE)的NdBa2Cu3O7-δ(NdBCO)高温超导厚膜作籽晶,通过冷籽晶熔融织构的方法生长YBa2Cu3O7-δ(YBCO)块体材料.与通常使用的籽晶相比,NdBCO厚膜籽晶具有如下优点:相对于非超导材料籽晶(MgO 等),NdBCO具有和YBCO相似的晶体结构和晶格常数,并对体系不会造成污染;与单晶体及熔融织构获得的籽晶相比,LPE获得的大尺寸NdBCO厚膜,有可能得到大单畴结构的YBCO块体材料;与NdBCO薄膜籽晶相比,NdBCO厚膜具有更高的结晶性能.本文讨论NdBCO厚膜籽晶生长YBCO块材过程中籽晶的影响及其热力学稳定性等问题.     

YBCO液相外延生长初始阶段的研究

通过液相外延生长的方法能制备高质量的YBa2Cu3O7-δ(YBCO)超导厚膜.利用高温金相显微镜,在大气气氛下实时观测了沉积在MgO基片上的YBCO薄膜熔化过程以及随后冷却过程中的液相外延生长初始阶段.通过对包晶分解过程的控制,留下部分微米级YBCO晶粒,并以此作为外延生长的种子.实验结果表明,通过包晶反应Y2BaCuO5+Liquid→YBa2Cu3O7-δ,能在这些剩余的YBCO晶粒周围快速外延生长出YBCO晶体.本文探讨了初始阶段的生长动力学以及外延生长取向问题.     

用电泳法在MgO基底上制备YBCO超导厚膜

电泳方法具有工艺简单,成本低廉,基底的形状和尺寸不受限制,膜厚容易控制的特点.本文采用电泳方法在00l取向的MgO基底上制备高温超导YBCO厚膜.在后退火过程中,采用籽晶诱导熔融生长法,成功制备转变温度约85K,转变宽度约3K的YBCO超导厚膜.X射线衍射结构分析揭示了在MgO基片上生长的样品绝大部分都是Y123相c轴取向的晶粒,少部分是Y211相的晶粒.此结果与通过扫描电子显微镜观察膜表面的形貌得到的结论是一致的.通过扫描电子显微镜的剖面图,可以看到生长非常清晰紧凑的,厚度约30μm的YBCO膜层.所制备YBCO厚膜样品用磁滞回线法估算其最高临界电流密度为0.978×103A/cm2,高于文献中用电泳法制备YBCO厚膜的最高临界电流密度.     

YBa2Cu3O7-δ薄膜厚度在多层异质结构(Ag/Ba0.1Sr0.9TiO3/YBa2Cu3O7-δ/LaAlO3)中对Ba0.1Sr0.9TiO3介电性能的影响研究

铁电/超导(Ba, Sr)TiO3/YBa2Cu3O7-δ异质结在可调谐微波器件方面具有非常好的应用前景.我们采用1.2°斜切LaAlO3基片,以脉冲激光沉积法(PLD)制备出性能较好的Ba0.1Sr0.9TiO3/YBa2Cu3O7-δ (BST/YBCO)异质薄膜.并进一步研究了YBCO薄膜厚度对BST性能的影响.研究发现当YBCO薄膜厚度增加到180nm附近时,其生长模式由二维step-flow转变为三维岛状模式,严重损害了在YBCO上面生长的BST薄膜的介电性能.具体表现在:BST薄膜的介电常数和可调谐率明显降低,介电损耗和漏电流却大幅度上升.通过测量电容与温度的关系,以应力效应模型对这一实验现象作出解释,认为YBCO薄膜厚度超过临界值,生长模式的转变促使晶格失配应力在YBCO和BST薄膜中得到释放,这导致BST/YBCO界面粗糙,以及BST薄膜中产生了大量的位错和缺陷,BST薄膜的性能因而大为降低.此外,通过对完全相同条件生长的单层YBCO薄膜的表面形貌进行了AFM研究,测试结果进一步验证了YBCO薄膜厚度增加到180nm时,其表面变得异常粗糙,均方根粗糙度(RMS)从120nm厚度时的3nm增加到180nm厚度时的9nm.因此,我们提出:通过严格控制底层YBCO薄膜的厚度,进而控制它的生长模式,能够非常有效地提高BST薄膜的介电性能.     

多源共蒸发制备高性能REBa2Cu3O7-x涂层导体的进展与展望

REBa2Cu3O7-x (RE：钇、钆等稀土元素,REBCO）高温超导体因其具备较高的不可逆场和上临界场等优越性能,一经发现就备受关注。但由于材料本身固有的陶瓷性及弱连接等属性,导致其实际应用起来难度较大。目前,人们已经发展了诸多制备工艺来克服这些困难,实现了REBCO超导体的实际应用。按照前驱膜沉积方法可将REBCO超导薄膜的制备分为物理法和化学法。本文综述了物理气相沉积（PVD-Physical Vapor Deposition）法中多源共蒸发法制备REBCO超导薄膜的技术起源及演变历程,并与金属有机沉积、金属有机化学气相沉积、脉冲激光沉积等不同方法生产的REBCO超导带材进行对比,突出多源共蒸发法制备的REBCO薄膜性能优异、在商业化生产效率上具有更大的优势。最后对多源共蒸发法制备REBCO超导薄膜进行总结及展望,解决多源共蒸发沉积制备REBCO薄膜的成相机理、提高薄膜的钉扎中心等问题对未来第二代高温超导带材的大规模应用具有重要意义。     

高氧压下氧化物薄膜同质和异质外延的RHEED实时监测

我们自行研制了具有三级差分气路可以在高气压下工作的RHEED系统(High-pressure RHEED),并利用本系统实时监测了(001)SrTiO3基片上SrTiO3:Nb、Ba0.5Sr0.5TiO3、YBa2Cu3O7单层薄膜,及Ba0.5Sr0.5TiO3/SrTiO3:Nb双层膜的生长过程.研究结果表明当镀膜室氧压高达21Pa时该系统仍然可以正常工作,并且能够获取较清晰的衍射图样.通过分析衍射图样我们发现,所有这些薄膜都是外延生长且晶体质量良好,但薄膜生长模式及表面平整度受沉积条件影响较大.在真空下薄膜基本上以层状模式生长,具备纳米级光滑的表面,且其表面平整度并不因膜厚的改变而变化;而在10Pa量级氧压下薄膜更倾向于以岛状模式生长,膜表面平整度较差,并且随膜厚的增加粗糙度上升.此外对多层薄膜而言,底层薄膜的表面和结构直接影响到顶层薄膜的质量和品质.     

关于YBCO薄膜过热现象的研究

在用YBa₂Cu₃O_z(YBCO)种膜液相外延生长Nd_1+xBa_2-xCuO_z(NdBCO)厚膜的过程中，YBCO晶体在高于熔点的温度下保持不熔化并且起到了外延种子的作用.采用高温金相显微镜,我们实时观察YBCO薄膜的熔化过程，发现了超导氧化物薄膜的过热现象，并且结合XRD极图的分析和Ba-Cu-O熔体的不润湿性现象合理解释了YBCO形成过热的机制.另外，通过对具有不同微观结构的YBCO薄膜熔化行为的横向比较，研究YBCO薄膜品质对于其过热度的影响，并用半共格界面能理论很好地解释了AFM和XRD分析及实时观察熔化过程的实验结果. 关键词： 过热 YBCO薄膜 熔化形核     

反应共蒸发法REBa_2Cu_3O_(7-δ)薄膜的异位成相过程研究

REBa_2Cu_3O_(7-δ)高温超导涂层导体是当前液氮温区载流能力最强的超导材料,它在大科学装置、军事国防、电力传输、磁悬浮列车等领域具有广泛应用潜力.按照薄膜沉积方式和成相步骤,超导层的制备技术路线可分为原位法(In-situ)和异位法(Ex-situ).本文将对异位法中的反应共蒸发法(RCE Reaction Co-evaporation)制备REBCO薄膜的物相形成规律进行研究,明确超导薄膜及其涂层导体在纳米级前驱组分、晶化温度调制下而形成的不同于块体体系的物相关系、织构生长特征.通过不同氧处理条件薄膜的组分和结构表征,获得了成相过程特征,发现较短的氧处理时间,"富稀土元素"组分等工艺设计有助于薄膜超导成相和c轴织构的形成.正REBa_2Cu_3O_(7-δ)(REBCO,RE=Y,Gd等稀土元素)高温超导涂层导体因其可克服晶界弱连接,高密度位错缺陷,进而提供强磁通钉扎且在液氮温区具有较高的载流能力和不可逆磁场成为倍受关注的热点材料.超导层的快速制备、厚膜织构的有效控制、磁场下的高临界电流密度以及制造成本的降低是第二代高温超导带材发展的关键问题[1-3].如今二代高温超导带材制备技术日趋成熟,主要分为物理法和化学法两大类[4],而按照其前驱膜     

用电泳技术制备YBCO高温超导厚膜

介绍了电泳技术制备YBCO高温超导厚膜的实验方法和YBCO高温超导厚膜的电学性质测量 ,讨论了在学生小型科研实验或设计实验中开展此实验的学时安排、注意事项和实验内容的扩展 .     

TFA-MOD法制备YBCO薄膜生长速率研究

采用原位电阻法对TFA-MOD法高温热处理阶段YBCO薄膜生长速率进行了研究。实验结果和分析表明原位电阻测量法是一种估算YBCO层生长速率的有效方法,不同条件下的测量结果表明薄膜生长速率随管式炉内的温度、水分压、气体流量的上升而明显增加,但随薄膜面积的增加而减小。实验结果为进一步探索和优化热处理过程提供了重要的基础。     

LPE growth of PZNT film using superheating YBCO thin film as seed layer

A superheating YBa₂Cu₃O_7-δ (YBCO or Y123) thin film was applied as a seed layer to grow Pb[(Zn_1/3Nb_2/3)_0.91Ti_0.09]O₃ (PZNT) films by a liquid phase epitaxy (LPE) process. In the present work, the YBCO thin film underwent a growth temperature of 1050 °C, which was about 40 °C higher than its peritectic temperature. It is very interesting that the superheated YBCO seed film could be used to grow not only Nd_1+xBa_2-xCu₃O_7-δ (NBCO) films with similar compositions but also PZNT films with completely different compositions. The XRD analysis confirmed that the PZNT film grown on the YBCO seeded MgO substrate had a good epitaxial relationship of [100](001)_PZNT//[100](001)_YBCO//[100] (001)_MgO. Compared with the PZNT films directly grown on MgO substrates, the LPE PZNT film on YBCO/MgO presented a better surface morphology. It was found that the superheating YBCO seed film plays a crucial role for the LPE growth of PZNT in the process. Furthermore, the superheating mechanism was discussed in terms of thermodynamic theories as well. PACS 77.84.-s; 61.10.Nz; 68.37.Hk; 81.15.Lm; 82.45.Mp     

In situ observation and simulation of growth process of faceted RE123 crystals

To clarify the growth mechanism of faceted REBa₂Cu₃O_7−δ (RE123, RE = Sm, Y) crystals, the growth process of the crystals was observed in situ by using a high temperature microscope. The growth rate of each faceted interface of a crystal growing from the liquid + 211 phases under an undercooling was obtained from the relationship between the position of each interface and growth time. It was observed that some of the faceted interfaces of a growing crystal stopped growing after a period of time, while other interfaces continued to grow with a growth rate approximated by a function of the undercooling. The above stoppage of the growth was observed in situ for the first time, and this fact could give powerful support to the mechanism for a similar phenomenon in REBCO films which were fabricated by the trifluoroacetates metal organic deposition method: growing microstructures of RE123 crystals in the film were revealed by transmission electron microscopy (TEM) for quenched specimens. Some very thin a-axis grains were formed by a change in c-axis growth rate. Furthermore, we showed the above growth and stop phenomena of faceted interfaces of REBCO crystal grains using numerical simulations.     

MgO粒子掺杂对NdBCO超导块材熔化温度的影响

采用改进后的顶部籽晶熔渗生长(RE+011 TSIG) 工艺, 通过在固相先驱粉中掺杂不同含量的 MgO 来有效地提高 NdBCO 籽晶的熔化温度, 从而成功地制备出直径为32 mm 的大尺寸单畴 SmBCO 超导块材. 结果表明,MgO 的掺杂对 NdBCO 超导块材的熔化温度有着明显的提高, 随着固相先驱粉中 MgO 掺杂量的增加, Mg2 + 离子逐渐进入到 Nd123 相的晶格中, 当掺杂量达到16 wt% 时呈现出饱和状态, 且 NdBCO 超导块材的熔化温度提高近18 ℃ , 可有效地抑制在制备SmBCO 超导块材的过程中出现的 NdBCO 籽晶熔化现象.     

Induced current of high temperature superconducting loops by combination of exciting coil and thermal switch

With its commercialization, the second-generation (2G) high temperature superconducting (HTS) RE—Ba—Cu—O (REBCO, RE is rare earth) tape is extensively applied to the superconducting magnets in the high magnetic fields. However, unlike low temperature superconducting (LTS) magnets, the HTS magnet cannot operate in the persistent current mode (PCM) due to the immature superconducting soldering technique. In this paper, an exciting method for two HTS sub-loops, so-called charging and load loops, is proposed by flux pump consisting of exciting coil and controllable thermal switch. Two HTS sub-loops are made of an REBCO tape with two slits. An exciting coil with iron core is located in one sub-loop and is supplied with a triangular waveform current so that magnetic field is generated in another sub-loop. The influence of magnetic flux on induced current in load loop is presented and verified in experiment at 77 K. The relationship between the induced magnetic flux density and the current on the sub-loops having been calibrated, magnetic flux density, and induced current are obtained. The results show that the HTS sub-loops can be excited by a coil with thermal switch and the induced current increases with magnetic flux of exciting coil increasing, which is promising for persistent current operation mode of HTS magnets.     

Fabrication of YBCO／YSZ and YBCO／MgO thick films using electrophoretic deposition with top-seeded melt growth process

Superconducting thick films were grown on single crystals MgO and YSZ by electrophoretic deposition with Y_2BaCuO_5(Y211) addition. YBCO thick films were then accomplished by sintering the precursor films above the peritectic temperature. Single crystals of MgO (3×3×0.5 mm^3) were used as top-seed to control crystal structure of the thick films. As shown by scanning electron microscopy, the morphologies of YBCO/YSZ and YBCO/MgO thick films are spherulitic texture and platelet type. The critical temperature is ～89 K for the YBCO/YSZ thick film; the onset transition temperature is 86.4 K and the transition width is ～3 K for YBCO/MgO thick film. The critical current densities (as determined by Bean model) are, in A/cm^2, 3870 (77 K) for YBCO/YSZ thick films and 2399 (77 K) for YBCO/MgO thick films, which are comparable to the best J_c reported of the thick films prepared by the same method.     

椭圆偏振光谱实时在线监测与离线分析微晶硅薄膜的生长

采用甚高频等离子体增强化学气相沉积技术高速沉积了有无籽晶层两个系列微晶硅薄膜,通过椭圆偏振光谱、拉曼光谱和XRD对薄膜进行了分析,发现采用籽晶层后,在薄膜沉积初期有促进晶化的作用;由于籽晶层减少了薄膜的诱导成核时间,提高了薄膜的沉积速率,对比了实时在线和离线椭圆偏振光谱两种测量状态对分析微晶硅薄膜的影响,研究发现,当薄膜较薄时,实时在线测量得到的薄膜厚度小于离线下的数值;当薄膜较厚时,两种测量条件下得到的薄膜厚度差异较小;实时在线条件下得到的表面粗糙度要大于离线条件下得到的数值,这是由于薄膜暴露在大气中后表面有硅氧化物生成,对表面有平滑作用.     

Top-seeded infiltration growth of Y–Ba–Cu–O bulk superconductors

A top-seeded melt-growth (TSMG) process is widely used to fabricate single domain YBa₂Cu₃O_y (Y–Ba–Cu–O) bulk superconductors. Pores are often found in the TSMG-processed Y–Ba–Cu–O samples due to the oxygen gas evolution during the molten stage. Recently developed liquid infiltration growth (LIG) process is known to be effective in suppressing the pore evolution and in refining the size of Y₂BaCuO₅ (Y211) particles dispersed in YBa₂Cu₃O_y matrix. The LIG process utilizes the liquid (Ba₃Cu₅O₈) infiltration into a pre- sintered Y211 contact and slow cooling through a peritectic temperature. In this study, we fabricated bulk Y–Ba–Cu–O superconductors by the LIG process combined with top-seeding with SmBa₂Cu₃O_y seed and confirmed that a single-domain bulk can be produced. Trapped field measurements however showed that some distortion in the field distribution was observed in the region near the seed crystal, which was attributed to Y211 density and its relatively large size.     

Features of the surface morphology of CaF<Subscript>2</Subscript>/Si(100) films obtained by solid-phase epitaxy

The dielectric parameters of calcium fluoride films grown on the Si(100) surface by solid-phase epitaxy (group 2) and without it (group 1) are analyzed. It is established experimentally that the deposition mode of CaF₂ films immediately after growth of the Si buffer layer at a substrate temperature of 530°C is not suitable for producing high-quality dielectric layers. The use of solid-phase epitaxy at the initial stage of the nucleation of CaF₂ layers enables the production of single crystal uniformly thick films with high dielectric properties.     

Scintillation efficiency and X-ray imaging with the RE-Doped LuAG thin films grown by liquid phase epitaxy

Very thin scintillator imaging plates have recently become of great interest. In high resolution X-ray radiography, very thin scintillator layers of about 5–20 μm are used to achieve 2D-spatial resolutions below 1 μm. Thin screens can be prepared by mechanical polishing from single crystals or by epitaxial growth on single-crystal substrates using the Liquid Phase Epitaxy technique (LPE). Other types of screens (e.g. deposited powder) do no reach required spatial resolutions. This work compares LPE-grown YAG and LuAG scintillator films doped with different rare earth ions (Cerium, Terbium and Europium). Two different fluxes were used in the LPE growth procedure. These LPE films are compared to YAG:Ce and LuAG:Ce screens made from bulk single crystals. Relative light yield was detected by a highly sensitive CCD camera. Scintillator screens were excited by a micro-focus X-ray source and the generated light was gathered by the CCD camera’s optical system. Scintillator 2D-homogeneity is examined in an X-ray imaging setup also using the CCD camera.