采用TFA-MOD技术在LaAlO3单晶基片上制备YBa2Cu3O7-x涂层导体

三氟乙酸盐-金属有机沉积技术（TFA-MOD）是制备钇钡铜氧涂层导体的有发展前景的方法之一。采用TFA-MOD技术在铝酸镧单晶基片上制备出YBa2Cu3O7-x涂层导体，并对不同烧结温度下制备的薄膜作了分析比较，找到了较为合适的烧结温度。用X射线衍射进行了物相的定性分析，由YBCO薄膜的（103）φ扫描图谱分析了薄膜的外延生长，用原子力显微镜观察了薄膜表面形貌。结果 表明制备出的YBCO薄膜表面均匀致密、无明显裂纹、有较强的（001）衍射峰。     

采用钙钛矿导电缓冲层提高YBCO涂层导体临界电流密度的可行性研究

以Ni合金为基底的YBCO涂层导体具有三明治结构,从下至上分别是:Ni合金、缓冲层、YBCO涂层与稳定层.在实用超导薄膜内部,局域超导电流由于晶粒弱连接、缺陷或裂纹等原因突然消失的情况下,一旦能量耗散超过临界值将会导致超导薄膜失超.在典型的YBCO涂层导体结构中,由于缓冲层是绝缘的氧化物,只能通过顶层的Ag或Cu稳定层的分流来实现电流传输方向的调整.如果在YBCO与正常金属基底之间存在连续的导体连接,即缓冲层导电,就可以不需稳定层,减少涂层导体的整体厚度,提高工程临界电流密度JE.如果钙钛矿导电缓冲层均匀无裂纹且足够厚,就可以起到隔离、外延、电流传输三重功效,同时提高JE.采用全化学溶液法制备了具有(00l)择优取向的BaPbO3,La0.5Sr0.5TiO3钙钛矿导电缓冲层与YBCO涂层,对于探索低成本的实用化工艺路线具有重要的实际应用价值.     

TFA-MOD制备YBCO带材工艺研究进展

由于第二代高温超导带材YBa2Cu3O7-z(简称YBCO)具有较高的不可逆磁场,可以在较高的温度和外加磁场下应用,是近年来高温超导材料研究的热点之一.采用三氟乙酸.金属有机沉积(trofluoroacetic acid-metal organic deposition,TFA-MOD)法制备第二代高温超导YBCO带材由于不需要真空系统,成本低,沉积速率快而广受关注.综述了TFA-MOD制备YBCO带材的工艺最新进展,并对TFA-MOD制备的YBCO带材性能进行了讨论.     

基带厚度对涂层导体立方织构Ni基带组织的影响

大变形量加工及随后再结晶热处理制备的立方织构Ni及其合金带材广泛用于YBa2Cu3O7-x(YBCO)涂层导体的基带。基带厚度的减小有利于提高涂层导体的工程电流密度。主要研究基带厚度对其立方织构、晶界角分布以及晶粒尺寸的影响。实验结果表明:随着基带厚度的减小,再结晶基带平均晶粒尺寸先减小后增大,当基带厚度为60μm时,晶粒平均尺寸达到最小值70μm;随基带厚度的减小,再结晶基带立方织构取向越接近其标准位置;晶界角分布随基带厚度变化不大,但所有样品晶界角几乎都小于15°。     

移动Ni-5W基带上制备钇系涂层导体隔离层的研究

采用电子束蒸发和磁控溅射两种工艺在移动的Ni-5W合金基带上制备了Y2O3隔离层,研究了镀膜过程中基带移动速度对隔离层性能的影响,同时详细比较了两种镀膜方法.利用扫描电镜、X射线衍射等手段对Y2O3隔离层进行了分析.结果表明:通过严格控制工艺条件,两种方法都能在移动Ni-5W合金基带上制备高立方织构、表面致密光滑的Y2O3隔离层.研究发现,电子束蒸发工艺中,理想的基带移动速度是0.4～1.0 mm·s-1;磁控溅射工艺中,适宜的基带移动速度应该是0.5～2.0mm·s-1.     

机械涂覆技术在功能涂层制备中的应用

机械涂覆技术在功能涂层制备方面,由于其设备简单,耗能低等特点,受到广大学者的青睐。目前,机械涂覆技术主要用于材料表面改性涂层和光催化涂层的制备,而两种涂层的形成和性能都受到多种因素的影响。因此,论述了机械涂覆技术的原理,并分别讨论了影响两种涂层形成和性能的影响因素,最后基于该技术目前在涂层制备中的限制,对未来的发展进行了展望。     

YBCO高温超导靶材制备工艺研究

进行了用钇钡铜氧（ＹＢＣＯ）系高温超导粉制备磁控和激光溅射超导薄膜用靶材的工艺研究。对靶材原料粉末的质量要求和制靶工艺进行了探讨，对影响靶材质量进而影响膜材质量的主要因素（如成分、纯度、均匀性、粒度及超导电性等）进行了研究。多家超导薄膜研究单位对本工艺靶材的使用结果证明了材料的优良品质，采用本工艺研制的大直径环形靶制出的超导薄膜，Ｊｃ值均在１０￣６Ａ／ｃｍ￣２水平。     

涂层导体用立方织构Ni基带的电化学抛光

大变形量加工及随后再结晶热处理制备的立方织构Ni及其合金带材广泛用于YBa2Cu3O7-x(YBCO)涂层导体的基带。隔离层及YBCO涂层的生长要求基带提供光滑的表面。但由于国内轧制水平的限制,轧制-再结晶基带的表面无法满足工艺使用的要求,必须通过表面处理改善基带表面质量。选用电化学抛光工艺提高基带表面质量,主要研究抛光液成分和抛光电流密度对抛光质量的影响。结果表明,磷酸含量85%,甘油含量15%,添加剂含量4 ml.L-1时,抛光效果最好。抛光后基带的最大表面粗糙度小于9 nm。     

静电喷涂涂层厚度的主要影响因素

本文主要从静电喷涂生产过程中的吊挂方式、工艺接地、喷涂轨迹、补粉方式、粉泵五个方面来阐述如何加强喷涂生产工艺控制，以便更加有效地提高喷涂涂层质量。     

Effect of humidity on microstructure and properties of YBCO film prepared by TFA-MOD method

Epitaxial YBCO superconducting films were deposited on the single crystal LaAlO3. (001) substrate by metal organic deposition method. All YBCO films were fired at 820 ℃ in humidity range of 2.6%-19.7% atmosphere. Microstructure of YBCO thin films was ana-lyzed by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). Superconducting properties of YBCO films were measured by four-probe method. XRD results showed that the second phase (such as BaF2)and a-axis-oriented grains existed in the films prepared at 2.6% humidity condition; a-axis-oriented grains increased in the film prepared at higher than 4.2% humidity condition; almost pure c-axias-oriented grains existed in the films fired at 4.2% humidity condition. Morphologies of the YBCO films showed that all films had a smooth and crack-free surface. YBCO film prepared at 4.2% humidity condition showed Jc value of 3.3 MA/cm2 at 77 K in self-field.     

化学溶液法在LaAlO3单晶基体上制备YBa2Cu3O7-x薄膜的研究

采用三氟乙酸盐-金属有机沉积(TFA-MOD)法在LaAlO3单晶基体上成功地制备了YBa2Cu3O7-x超导薄膜(简称YBCO薄膜),并比较系统地研究了烧结温度对YBCO薄膜的影响。在烧结温度为820℃时,所制备的YBCO薄膜完全呈c-轴取向,无a-轴取向的晶粒和杂质相存在,YBCO薄膜的表面无裂纹存在,表面平整,超导转变温度Tc≈90K,转变宽度ΔTc=1K,临界电流密度(Jc)可达1.2MA.cm-2(77K,0T)。     

TEM Analysis on YBCO Composited Superconducting Tapes

The microstructures of the YBCO composited superconducting tapes with different J_c were analysed byTEM.The relationship between microstructure and J_c of the tapes is discussed in detail.It is demonstrated thatJ_c value of the tapes increases significantly with the decrease in the width of grain boundary,increase of the twindensity and the reducing of the amount of precipitates at grain boundary.At grain boundary of the tapes,howev-er,small amount of non-superconducting phases can-not be avoided.For the fabrication of high J_c YBCO com-posited tapes,it is very important to improve the microstructure of the superconductor perfectly.     

热处理温度对MOD-YBCO薄膜微结构和超导电性的影响

采用TFA-MOD法在LaAlO3基体上制备YBCO薄膜,热处理温度为780-860℃。XRD结果表明,热处理温度在780-820℃之间时,随着热处理温度的提高,YBCO薄膜中BaF2逐渐减少,a轴生长的晶粒和杂质相减少,c轴生长的晶粒增加;热处理温度在820-860℃之间时,随着热处理温度的升高,薄膜中a轴生长的晶粒增加,c轴生长的晶粒减少;SEM分析发现,YBCO薄膜表面较平整,无裂纹;超导性能测试结果表明,热处理温度为820℃的YBCO薄膜的临界电流密度Jc可达1 MA.cm^-2（77 K,0 T）。     

Preparation of high performance YGdBCO films by low fluorine TFA-MOD process

YBCO films doped with different contents of gadolinium(Gd) were prepared by the low-fluorine(low-F)trifluoroacetate metal-organic deposition(MOD) method.The effects of flow rate and holding time of the firing(crystallization) stage on the superconducting properties of Y_xGd_(1-x)Ba_2 Cu_3 O_(7-δ)(YGdBCO) films were investigated.The phase formation and texture were characterized by the X-ray diffraction(XRD),which indicate that severe degradation of the microstructure will be induced with the inappropriate flow rate.The surface morphology and element distribution were investigated by the scanning electron microscopy(SEM) and energy dispersive spectroscopy(EDS).The results show that increasing the holding time of the firing stage is effective for the further decomposition of residual impurity phase on the surface.The mechanisms of the phase and surface evolution are also discussed.Finally,a high critical current density(J_c) value of 5.4 MA/cm~2 was achieved in the Y_(0.9)Gd_(0.1)BCO film fabricated by the cooperative control of the flow rate and holding time of the firing stage,which are contributed to the formation of excellent texture,homogeneous microstructure and dense surface of the YGdBCO films.     

Fabrication of NiO Buffer Layer for YBCO Coated Conductors by Combining Sputtering and SOE Method

In research of YBCO coated conductors, the development of a oxide template for epitaxial growth of YBCO is very important. Matsumoto et al have demonstrated the potential of the surface oxidation epitaxial (SOE) route for formation a cube textured NiO layer on nickel tapes. The epitaxial NiO functions as a buffer layer of chemical reaction between YBCO and nickel, and as a template for the epitaxial growth of YBCO. However, the surface quality of NiO is difficult to control and defects such as crack, spall and deep grooves exist in SOE NiO layer. A new approach combining sputtering and SOE method to obtain crack-free and cube textured NiO layer were reported. Ni tapes prepared by the combination of rolling and recrystallization were used for this work. A coating of Ni was first deposited on the tapes via magnetron sputtering. Then on the coating tapes, continuous and textured NiO layer were achieved by SOE technology.     

射频溅射法在CeO2/YSZ/Y2O3/NiW衬底上制备YBCO超导层

用射频溅射的方法在强立方织构的CeO2/YSZ/Y2O3/NiW衬底上制备了YBCO超导层. 温度、气压等因素对超导层的外延生长有重要影响. 在基片温度大于780 ℃, 气压在11～160 Pa之间, 都有NiWO4化合物生成;在退火吸氧过程中, 金属基底被氧化. 最终在温度780 ℃, 气压100 Pa的条件下, 制备出了纯（00l）取向的YBCO薄膜, 其平面内φ扫描半高宽小于10°, 超导转变温度为87.2 K, 传导电流为11 A.     

磁控溅射制备YBCO超导薄膜的AFM研究

采用中空柱阴极直流磁控溅射装置制备YBCO超导薄膜,应用原子力显微镜（AFM）研究了在最佳工艺条件下沉积在LaAlO3和Zr(Y)O2上的具有c轴取向的YBCO超导薄膜及其相应衬底的表面形貌,生长的YBCO膜都具有较好的表面结构,在LaAlO3单晶衬底上的YBCO膜形成大颗粒岛状结构,颗粒生长整齐,尺寸大小均匀;生长在单晶Zr(Y)O2上的YBCO膜则形成起伏较大的层状与岛状生长的混合结构,这些差别的产生与衬底的初始状况及制备过程中膜与衬底的界面作用有关。分析了形成超导薄膜不同表面形貌的原因,从生长机理角度讨论了表面形貌与缺陷和位错的形成机制。