Nb5+掺杂对低氟MOD法制备的YBCO薄膜性能的影响

本研究通过低氟MOD法成功地制备了Nb⁵⁺掺杂的YBa₂Cu₃O_7-x(YBCO)薄膜, Nb⁵⁺在薄膜中生成了大小在20~30 nm之间的纳米颗粒; 纳米颗粒的生成不会对 YBCO薄膜的织构和临界温度(T_c)构成明显的影响。由于纳米颗粒的引入, 掺杂后薄膜的临界电流密度(J_c)在整个磁场范围内都要高于纯的YBCO, 自场下的Jc更是达到了3.4 MA/cm²。掺杂薄膜的钉扎力(F_p)也远远大于纯YBCO, 最大钉扎力达到了3.25 GN/m³, 有效地提高了YBCO在外加磁下的超导性能。     

提高YBCO薄膜高场性能的研究

采用低氟的金属有机盐沉积技术(MOD)在LAO单晶上制备了Gd和Zr掺杂的YBCO薄膜, 并分析了不同掺杂对YBCO薄膜在外加磁场下的Jc的影响. 研究发现, 采用Gd部分取代YBCO薄膜中的Y元素, 可以有效地提高YBCO薄膜高场下的J_c值, 但对于低场下的Jc值影响不大; 而采用过量Gd掺杂YBCO薄膜, 可以有效地提高YBCO薄膜在低场下的J_c值, 但对于高场下的J_c值影响不大. 而Zr掺杂可以有效地提高YBCO薄膜在低场和高场下的J_c值. 最后, 结合Gd取代和Zr掺杂两种方式, 有效地提高了YBCO薄膜的场性能, 其最大钉扎力(Fp(Max))达到了16GN/m³, 比纯的YBCO薄膜(4.0 GN/m³)提高了约3倍; 在磁场为3T和7T下, 其J_c值分别为1.31MA/cm²和87.7kA/cm².     

Nb掺杂YBCO薄膜钉扎机理的研究

通过低氟MOD法制备了Nb掺杂的YBa₂Cu₃O_7-x(YBCO)薄膜, 掺入的Nb以Ba₂YNbO₆(BYNO)相存在, 其尺寸大小在20~30 nm之间, 薄膜中BYNO纳米颗粒以外延和随机两种取向共存, 且以随机取向为主。BYNO纳米颗粒的周围出现堆垛层错, 并且BYNO周围的YBCO出现严重的晶格畸变, 这增加了YBCO薄膜内部的微观应变, 且随机BYNO颗粒含量越高, YBCO薄膜内部的微观应变就越大。微观应变增加了薄膜的磁通钉扎能力, 进而提高了薄膜在高磁场下的超导性能。     

柔性Eu3+掺杂SiO2纳米纤维薄膜的制备及其发光性能

采用溶胶-凝胶法结合静电纺丝技术制备了柔性Eu³⁺掺杂SiO₂纤维薄膜, 采用SEM、XRD、FT-IR、TG和PL等测试方法对材料进行表征。Eu³⁺掺杂SiO₂纤维薄膜在热处理后纤维直径变小, 纤维表面平滑无粘连。通过控制升温速度, 纤维薄膜经热处理后仍具有较高的力学强度, 750℃热处理后其拉伸强度可达4.31 MPa, 经过多次弯曲仍能保持原样。在392.6 nm光源激发下, Eu³⁺掺杂SiO₂纤维薄膜在570~670 nm附近呈现出来自于⁵D₀→⁷F_J的发射峰。当Eu³⁺掺杂浓度为8mol%时, 经过750℃热处理后Eu³⁺掺杂SiO₂纤维薄膜的发光强度达到最大值。     

Pr掺杂Mg2SnO4纳米颗粒的制备及其光致发光性能

采用水热合成和低温煅烧两步法工艺制备了不同浓度(0~1.5mol%)镨掺杂锡酸镁, 通过X射线衍射(XRD)、扫描电子显微镜(SEM)及荧光光谱仪对合成的样品进行表征, 研究了Pr掺杂量对锡酸镁微观形貌的影响, 并讨论了其光致发光性能。结果表明, 所制备的Mg₂SnO₄: Pr³⁺为立方反尖晶石结构的立方纳米颗粒; 与未掺杂的Mg₂SnO₄相比, Pr掺杂浓度的增加使颗粒尺寸变大, 并使颗粒边角锐化。不同浓度Mg₂SnO₄: Pr³⁺的发射光谱表明Mg₂SnO₄: Pr³⁺样品中存在530、570 nm两处发射峰, 前者与Mg₂SnO₄基质中的氧空位有关, 后者由Pr元素³P₀-³H₅能级的跃迁造成。随着Pr掺杂浓度增加, 锡酸镁颗粒尺寸变大、发光中心增多, 使得Pr掺杂锡酸镁纳米颗粒在570 nm处的发光强度增强。     

MOD方法制备Y0.5Yb0.5BCO薄膜及其性能研究

采用低氟金属有机物沉积工艺, 通过将浓度相同的YBCO、YbBCO前驱溶液按1: 1的体积比混合, 使元素Yb部分取代Y, 成功制备了Y_0.5Yb_0.5BCO薄膜. 该薄膜成份单一, 具有很好的双轴织构; 薄膜表面平整致密, 没有裂纹和孔洞, 元素分布均匀. 虽然Yb部分取代Y降低了薄膜的临界转变温度(T_c), 但有效提高了薄膜在高场下的场性能, 如在77K, 3T磁场下, Y_0.5Yb_0.5BCO薄膜的J_c值提高了1.26倍. 为了进一步改善薄膜在低场下的性能, 通过在Y_0.5Yb_0.5BCO前驱溶液中再加入6 mol%的TaCl₅, 成功地制备了Ta⁵⁺掺杂的Y_0.5Yb_0.5BCO薄膜, 提高了薄膜在整个磁场范围内的载流能力.     

Ag-SiO2-CeF3：Tb3+复合纳米粒子的制备与发光性质

采用简单的液相法在室温下制备了均匀球形的Ag-SiO₂-CeF₃：Tb³⁺核-壳结构纳米复合发光粒子,并对其结构和性能进行了表征。测试结果表明：Ag-SiO₂表面包覆上了结晶良好的六方晶系的CeF₃：Tb³⁺。Ag-SiO₂-CeF₃：Tb³⁺纳米复合粒子为球形,尺寸约为45~60 nm,该纳米复合粒子与CeF₃：Tb³⁺一样具有良好的特征绿光发射,均以544 nm附近的Tb³⁺的⁵D₄→⁷F₅跃迁为最强发射峰,内核贵金属Ag纳米粒子对CeF₃：Tb³⁺发光起到了一定的猝灭作用。Ag-SiO₂-CeF₃：Tb³⁺复合材料在生物检测、疾病治疗方面具有潜在的应用。     

介孔氧化硅/氧化铈核壳双相复合颗粒的制备及其光催化降解活性

将CeO₂纳米粒子负载在介孔氧化硅(W-mSiO₂)支撑体上,制备了核壳结构的W-mSiO₂/CeO₂双相光催化复合颗粒。用X射线衍射、扫描电镜、透射电镜、氮气吸脱附、STEM-EDX mapping、Raman光谱、荧光光谱、紫外-可见漫反射光谱等手段分析样品的结构和性质,考察了复合光催化材料对亚甲基蓝(MB)的光催化降解反应活性。结果表明,复合颗粒中介孔氧化硅内核的尺寸为180~200 nm、比表面积高达1627 m²/g,包覆层(厚度约20 nm)由大量尺寸为数纳米的氧化铈粒子组成。介孔内核对MB有较强的吸附能力,使之富集在CeO₂活性粒子周围,从而提高了复合颗粒对MB的光催化降解效果。对壳层CeO₂纳米粒子进行Er³⁺掺杂改性并在非氧化性气氛(氮气)中保护煅烧,有助于进一步提高复合颗粒对MB的光催化降解活性。     

低氟MOD法制备Zr掺杂YBCO薄膜的研究

在金属有机盐沉积（MOD）法制备YBCO薄膜的工艺中, 采用无F的α甲基丙烯酸铜取代原来的三氟乙酸铜, 可以降低前驱溶液中大约50%的氟含量. 研究表明, 该方法大大缩短了YBCO前驱薄膜受热分解的时间, 仅为原来的1/7. 通过XRD、SEM分析发现, 该方法可以制备成分单一、具有良好立方织构的YBCO薄膜, 且薄膜表面平整致密, 没有裂纹, 临界温度(T_c)达到了90K左右, 77K、自场下的临街电流密度(J_c)达到了2.84MA/cm². 通过在制备的YBCO薄膜中引入6mol% 的 Zr元素掺杂, 有效地提高了YBCO薄膜在外加磁场下的超导性能.     

Nd3+掺杂的NaYF4:Yb@NaYF4:Ho上转换纳米颗粒的光谱分析

上转换纳米颗粒因具有良好的穿透深度和发光强度被广泛地应用在生物标记或生物成像中。实验制备了核壳结构的NaYF₄:Yb@NaYF₄:Ho纳米颗粒, 分散均匀, 粒径在50 nm左右。通过光谱分析可知, 该纳米颗粒可在980 nm激光激发下发射波长为650 nm为主的发射光。进一步对该核壳结构的NaYF₄:Yb@NaYF₄:Ho纳米颗粒进行Nd³⁺掺杂, 制备了可被800 nm激光激发且发射强红光的纳米颗粒。通过比较多种不同结构的Nd³⁺掺杂NaYF₄:Yb@NaYF₄:Ho纳米颗粒的荧光光谱发现, NaYF₄:Yb@NaYF₄:Ho,Nd纳米颗粒发射光最强, 表明Nd³⁺掺杂在NaYF₄:Yb@NaYF₄:Ho纳米颗粒的壳层中最佳。最后对NaYF₄:Yb³⁺50%@NaYF₄:Ho³⁺1%,Nd³⁺x%纳米颗粒Nd³⁺离子的掺杂浓度进行优化, 实验结果表明: Nd³⁺掺杂浓度为30%时,该纳米颗粒在800 nm激光激发下发光强度最强。     

Preparation and characterization of YBa2Cu3O7−x high Tc superconducting thin films deposited by S-gun sputtering

We have prepared YBa₂Cu₃O_7−x high T_c superconducting (HTS) thin films on (100) yttria-stabilized zirconia (YSZ) and LaAlO₃ (LAO) substrates, using a 2 kW S-gun in an off-axis mode. By varying the temperature of the substrates, films with a axis and c axis orientations were readily obtained. The X-ray diffraction pattern and Laue pattern confirmed that films with a axis orientation exhibited a single-crystal texture. All films had a good mirror-like surface. For films grown on YSZ substrates, scanning electron microscopy (SEM) revealed a clear distinction between the surfaces of the films grown at various temperatures (520–780°C). Films grown on LAO substrates exhibited even smoother and flatter surfaces. The SEM changes will be discussed in correlation with J_c. The best HTS thin films were obtained on LAO substrates at a temperature of 820°C, with T_c=89 K and J_c=1×10⁶ A cm^-2 (77 K).     

Thermomechanical processing and transport current density of Ag-sheathed (Tl,Cr)Sr2(Ca0.9,Pr0.1)Cu2O7 superconductor tapes

Powders with nominal composition (Tl,Cr_0.15)Sr₂(Ca_0.9,Pr_0.1)Cu₂O₇ (Tl-1212) and T_c90 K were used to fabricate Ag-sheathed superconducting tapes employing the powder-in-tube (PIT) method. The tapes were subjected to intermediate mechanical rolling or pressing. Conditions that enhance the transport critical current density (J_c) of the tapes were investigated. Optimum annealing temperature and period together with uniaxial pressing are necessary to increase J_c of the Tl-1212/Ag tapes. Annealing at 910 °C for 0.5–1 h enhanced the 1212 phase formation and improved intergranular connectivity between grains, as well as to provide healing for the fractured structure caused by deformation process. A relatively longer annealing time at higher temperature gave rise to secondary phases and resulted in the decrease of J_c. Mechanical uniaxial pressing greatly densified the tapes core and thus led to closer contact between grains. At liquid nitrogen temperature and zero field, J_c of the pressed tapes annealed at 910 °C for 1 h is 3060±127 A cm⁻². The initial drastic drop of J_c in low fields (<0.06 T) indicates the performance of the tapes is limited by weak links. No significant anisotropic transport properties were observed in applied magnetic field. This is due to the absence of texturing in the tapes as the grains are randomly oriented revealed through SEM micrographs.     

温度控制织构金属基带上YBCO外延薄膜生长及缺陷研究

采用直流溅射法在Y₂O₃/YSZ/CeO₂(YYC)缓冲层的织构NiW基带上, 通过基片温度调制YBa₂Cu₃O_7-δ(YBCO)外延薄膜生长。X射线衍射仪(XRD)表征显示, 基片温度强烈地影响YBCO薄膜的外延生长: 在较低的基片温度下薄膜趋于a轴取向生长, 随基片温度升高薄膜逐渐变为纯c轴取向生长。由于a轴晶粒引起的大角度晶界会阻碍超导电流在a-b面内的传输, 因此YBCO薄膜的微观结构和超导电性能随温度升高而得到改善, 但是随着基片温度继续升高, 基带的氧化程度加剧, YBCO与缓冲层间发生界面反应, 从而导致薄膜质量衰退。本     

Ba源配比对MOCVD法制备YBCO薄膜性能的影响研究

采用单一液相混合源进液及闪蒸的MOCVD系统在LaAlO₃(001)单晶基片上制备YBa₂Cu₃O_7-x(YBCO)薄膜, 研究混合源中Ba含量对YBCO超导薄膜成分、结构及电流承载能力的影响。结果表明, 当Ba含量较小时, YBCO薄膜中易于形成尺寸较小的CuO颗粒; 随着Ba含量的增加, 薄膜中形成Ba₂CuO₃晶粒, 并且Ba₂CuO₃晶粒尺寸随Ba含量的增加而逐渐增大。杂质相的含量、尺寸以及与YBCO的晶格匹配程度对YBCO薄膜的双轴取向生长和电流承载能力具有重要影响。当原料摩尔配比Ba/Y=3.9时, 成功制备出了具有优异面内面外取向、结构致密的YBCO超导薄膜, 77 K下的300 nm厚度薄膜的临界电流密度达到4.0 MA/cm², 该研究结果对于第二代涂层导体的发展具有重要意义。     

Influence of Interfacial LSMO Nanoparticles/Layer on the Vortex Pinning Properties of YBCO Thin Film

YBa₂Cu₃O_7?δ (YBCO) thin films have been deposited on bare and La_0.67Sr_0.33MnO₃ (LSMO) modified single crystal SrTiO₃ (STO) substrates. The effect of randomly distributed ferromagnetic LSMO nanoparticles and a complete LSMO layer, present at STO/YBCO interface, on the superconducting properties of YBCO thin films has been investigated by temperature dependent magnetization studies. The YBCO thin film on LSMO nanoparticles decorated STO substrate shows significant improvement in the critical current density and pinning force density as compared to the YBCO thin film deposited on bare STO substrate and this improvement is more significant at higher applied magnetic field. However, the LSMO/YBCO bilayer showed the improved flux pinning properties only up to a magnetic field of 1.5 T above which it deteriorates. In the case of LSMO/YBCO bilayer, the underlying LSMO layer gives rise to magnetic inhomogeneities due to domain structure, which leads to improved flux pinning properties limited to lower field. However, in the case of LSMO nanoparticles decorated substrate, the presence of LSMO nanoparticles at YBCO/STO interface seems to introduce magnetic inhomogeneities as well as structural defects, which might be acting as correlated pinning sites leading to improved flux pinning properties of the YBCO thin film over a wide range of applied magnetic field.     

Determination of the fracture toughness of fabric reinforced composites by the J-integral approach

The fracture behaviour of a glass-fabric-reinforced epoxy composite has been investigated experimentally. Load-displacement curves for single-edge-notched specimens were obtained on an MTS system and the J-integral evaluated through its energy rate interpretation. J_c, the critical value of the J-integral, obtained directly for a₀/w > 0·4 and that obtained through an extrapolation procedure for a₀/w < 0·4 compare quite well. J_c appears to be independent of crack length for specimen widths between 15 and 45 mm. J_c for ±45° specimens is less than half that for 0/90 specimens.     

Comparison of Flux Pinning Mechanism in Laser Ablated YBCO and YBCO:BaZrO3 Nanocomposite Thin Films

Thin films of YBCO and YBCO:BaZrO₃ (BZO) nanocomposite have been deposited using the pulsed laser deposition technique. Substantial increase in critical current density (J _C ) and pinning force density (F _p ) of the nanocomposite thin films was observed. The possible pinning mechanism in YBCO:BZO nanocomposite thin films has been explored and compared with the pinning mechanism in pure YBCO thin film by studying the variation of J _C with magnetic field (B) and temperature. In the intermediate field regime (0.1–1 T), J _C follows B ^−α with nearly similar values of α for YBCO and YBCO:BZO nanocomposite thin films indicating similar pinning mechanism in both thin films. The variation of J _C with reduced temperature (t=T/T _C ) has been studied for both the films and it was observed that the mechanism of pinning in both YBCO and YBCO:BZO thin films is similar (δT _C pinning). The observed enhanced values of J _C and F _p of the nanocomposite thin film is attributed to the presence of BZO nanoparticles, which induces more defects due to lattice mismatch between YBCO and BZO leading to improved flux pinning properties of the nanocomposite thin film.     

Pd/PMo12-GN复合膜的制备及其对甲酸氧化的电催化性能

以紫外光还原法将氧化石墨(GO)还原成石墨烯(GN), 同时将磷钼酸(PMo₁₂)修饰到石墨烯上, 形成磷钼酸功能化的石墨烯PMo₁₂-GN, 并以此为基底利用电化学还原法制备了Pd/PMo₁₂-GN复合膜催化剂。运用X射线粉末衍射、X射线光电子能谱、扫描电镜、透射电镜等对复合膜的组成、结构、形态进行表征, 结果表明: 实验成功制备了Pd/PMo₁₂-GN复合膜催化剂, 且Pd颗粒均匀分散在PMo₁₂-GN基底上。采用CV、计时电流法、CO溶出伏安法、交流阻抗法等电化学方法研究了Pd/PMo₁₂-GN复合膜的电催化性能。研究结果表明: 制备的复合膜催化剂对甲酸氧化反应的催化活性、催化稳定性、抗CO毒化能力和电子传递能力显著优于商品化的Pd/C催化剂。Pd/PMo₁₂-GN复合膜电催化性能的提高主要是由于Pd纳米颗粒在PMo₁₂-GN基底上均匀分散, 以及PMo₁₂的强氧化能力从而使钯表面一氧化碳等中间产物能迅速氧化去除。