H, C, N NMR, ESI mass spectral and single crystal X-ray structural characterization of three spiro[pyrrolidine-2,3′-oxindoles]

Three spiro[pyrrolidine-2,3′-oxindoles], 1,1′,2,2′,5′,6′,7′,7′a-octahydro-2-oxo-1′-phenyl-spiro[3H-indole-3,3′-[3H]-pyrrolizine]-2′-carboxylic acid methyl ester (1), 1,1′,2,2′,5′,6′,7′,7′a-octahydro-2-oxo-1′-nitro-2′-phenyl-spiro[3H-indole-3, 3′-[3H]-pyrrolizine] (2) and 1,1′,2,2′,5′,6′,7′,7′a-octahydro-2-oxo-1′-nitro-2′-(4″-chlorophenyl)-spiro[3H-indole-3,3′-[3H]-pyrrolizine] (3) have been synthesized and their ¹H, ¹³C and ¹⁵N spectra assigned. The chemical shift assignments are based on Pulsed Field Gradient (PFG) Double Quantum Filter (DQF) ¹H, ¹H correlation spectroscopy (COSY), PFG ¹H, ¹³C Heteronuclear Multiple Quantum Coherence (HMQC) and PFG ¹H,X (X = ¹³C and ¹⁵N) Heteronuclear Multiple Bond Correlation (HMBC) experiments. The single crystal X-ray structures of 1–3 have been determined. Compounds 1 and 2 crystallized in monoclinic space group C2/c and compound 3 in monoclinic space group P2₁/c, respectively. Also the ESI-TOF MS data of 1–3 are given.     

[Mn(H_2O)_4(NCS)_2)(18C6)和(Co(H_2O)_4(NCS)_2)(18C6)单晶的培养及物性表征

用凝胶法和蒸发法分别培养出配合物[Mn(H_2O)_4(NCS)_2]18C6)和[Co(H_2O)_4(NCS)_2](18C6)的单晶。对两个配合物进行了溶解性能的测试、元素分析、电导测量、红外光谱分析、热分析和质谱分析。表征的指派为晶体结构分析结果所证实。 。。     

Influence of the variable wall thickness of the sample tubes and a quartz Dewar on the EPR signal intensity in a single TE102 and double TE104 rectangular cavity

The response of a single TE₁₀₂ and double TE₁₀₄ rectangular cavity to the insertion of samples contained in tubes with variable wall thickness and a quartz Dewar into the cavity has been analyzed. A direct, indirect, and concurrent (positive or negative) “lens effect” inside the double TE₁₀₄ rectangular cavity is discussed. The experimental dependence of the EPR signal intensity on the wall thickness of the sample tube, δ, for the line-like samples with identical length of the sample material column, L=30 mm, recorded in the microwave cavity showed a directly proportional increase of the relative “lens effect” with the increase of the wall thickness of the tube in the interval, δ∈<0.1 mm, >0.5 mm. The insertion of the variable-temperature double-wall quartz Dewar (home-built, resonant frequency shift, ca. −300 MHz) into the single TE₁₀₂ rectangular cavity showed the same relative “lens effect”, with ca. 1.5-time increase of the EPR signal intensity, for a point-like sample and the line-like samples with material columns of diameter of 1 and 1.3 mm, and wall thickness of the sample tubes, δ∈<0.1 mm, >0.5 mm. The increased effect of the Dewar arises because the active volume of the quartz Dewar tube walls is always much more larger than the active volume of the sample tube wall. In the case of the double TE₁₀₄ rectangular cavity, the insertion of the quartz Dewar: (i) into the same cavity, in which the sample is present, caused a direct “lens effect”, with ca. 1.8-fold increase of the EPR signal intensity; however, (ii) into the complementary cavity, in which the sample is absent, caused an indirect “lens effect”, with ca. 0.6-fold decrease of the EPR signal intensity. With the Dewar and sample in one cavity and a large empty sample tube in the complementary cavity, a concurrent (positive or negative) “lens effect” can be observed. Thus, the possible increase/decrease of the EPR signal intensity depends on the volume ratio of the quartz Dewar tube walls and large sample tube wall inserted into the double TE₁₀₄ rectangular cavity. Each of the above phenomena may be a significant source error in quantitative EPR spectrometry unless the samples to be compared in the quantitative EPR analysis are contained in sample tubes having the same wall thickness and each EPR spectra should be recorded inside an identical quartz Dewar.     

Characterisation of electroplated Sn/Ag solder bumps

Environmental concerns as well as legal constraints have been pushing research on flip chip technology towards the development of lead-free solders and also to new deposition techniques [Z.S. Karim, R. Schetty, Lead-free bump interconnections for flip-chip applications, in: IEEE/CPMT 1nternational Electronics Manufacturing Technology Symposium, 2000, pp. 274-278, P. Wölflick, K. Feldmann, Lead-free low-cost flip chip process chain: layout, process, reliability, in: IEEE International Electronics Manufacturing Technology (IEMT) Symposium, 2002, pp. 27-34, M. McCormack, S. Jin, The design and properties of new, pb-free solder alloys, in: IEEE/CPMT International Electronics Manufacturing Technology Symposium, 1994, pp. 7-14, T. Laine-Ylijoki, H. Steen, A. Forsten, Development and validation of a lead-free alloy for solder paste applications. IEEE Transactions on Components, Packaging, and Manufacturing technology, 20(3) (1997) 194-198, D. Frear, J. Jang, J. Lin, C. Zhang, Pb-free solders for flip-chip interconnects, JOM, 53(6) (2001) 28-32].Binary and ternary tin alloys are promising candidates to substitute lead-content components. In this paper, we describe an electroplating technique for high density FlipChip packaging [M. Bigas, E. Cabruja, Electrodeposited Sn/Ag for flip chip connection, CDE (2003)]. An analysis using Auger Electron Spectroscopy (AES) together with additional Energy Dispersive Xray analysis (EDS) tests and Scanning Electron Microscope (SEM) analysis have been performed to optimize the reflow process of the electrodeposited bumps.     

微流控芯片分析系统中硅胶整体柱和膜滤复合预处理单元的构建

以改性C18反相硅胶整体柱为微流控芯片分析系统中固相萃取介质材料, 构建不同功能单元的样品预处理微分析系统, 实现了血清样品中痕量盐酸多巴酚丁胺的富集. 初步构建了单一改性硅胶微柱固相萃取预处理单元, 测试得到了改性硅胶整体柱对血清中痕量盐酸多巴酚丁胺的平均富集倍数为77.2, RSD为12.35％. 为了提高测试的精密度, 进而设计含膜复合式预处理芯片, 探讨了不同预处理单元对血清样品中痕量盐酸多巴酚丁胺富集效率的影响, 优化设计了外接式硅胶整体柱-亲和膜微芯片固相萃取预处理单元, 复合式的反相硅胶整体柱对血清中微量盐酸多巴酚丁胺的平均富集倍数提高到89.4, RSD为4.37％. 结果显示了该预处理单元在血清中痕量药物富集的可行性和有效性.     

基于侧向磁泳的微流控芯片对两种磁性纳米球的同时分选

基于磁性纳米球在微流控芯片上的侧向磁泳,利用微流控芯片分选了不同磁响应性的磁球.提出了包含磁性纳米球聚集与偏移的理论模型,用于分析磁球在芯片上的侧向位移.在理论分析的基础上设计了芯片系统,使不同磁响应性的磁纳米球可以在芯片系统上依次被分选.实验结果表明,2种磁性纳米球的分选效率均可接受,且实验操作简单;磁响应性强的磁球可被完全分离,这对于珍贵分析样品的分选很有价值.该分选系统被成功用于同时分选样品中乙型肝炎病毒的DNA与丙型肝炎病毒的反转录DNA,在生化分析中具有广阔的应用前景.     

可拉伸超韧水凝胶的制备和应用

综述了可拉伸超韧水凝胶的设计原理及其在组织工程和柔性电子器件领域的应用.通过将网络结构层次、化学结构、增韧机制与宏观力学性能相结合,重点讨论了单网络水凝胶、双网络水凝胶、纳米复合水凝胶及其它水凝胶等可拉伸超韧水凝胶的研究进展,并总结和展望了新思路和新方向.     

注入锁定激光器的边带锁频技术稳频系统优化分析

介绍了边带锁频技术稳频方法,推导出鉴频曲线,对稳频控制过程进行了分析.建立了注入锁定激光器的边带锁频技术稳频系统理论模型,讨论了相关参量对稳频效果的影响并且进行了优化.结果表明,增加入射光强,采用窄线宽的法布里-珀罗以及对法布里-珀罗进行高准确度温控都可以增强稳频效果.提出适用于注入锁定激光器的两种稳频方案并进行比较.     

基于四值脉冲参数模型的单粒子瞬态传播机理与软错误率分析方法

随着工艺尺寸的不断缩小,由单粒子瞬态(Single Event Transient, SET)效应引起的软错误已经成为影响宇航用深亚微米VLSI电路可靠性的主要威胁,而SET脉冲的产生和传播也成为电路软错误研究的热点问题。通过研究SET脉冲在逻辑链路中的传播发现：脉冲上升时间和下降时间的差异能够引起输出脉冲宽度的展宽或衰减;脉冲的宽度和幅度可决定其是否会被门的电气效应所屏蔽。该文提出一种四值脉冲参数模型可准确模拟SET脉冲形状,并采用结合查找表和经验公式的方法来模拟SET脉冲在电路中的传播过程。该文提出的四值脉冲参数模型可模拟SET脉冲在传播过程中的展宽和衰减效应,与单参数脉冲模型相比计算精度提高了2.4%。该文应用基于图的故障传播概率算法模拟SET脉冲传播过程中的逻辑屏蔽,可快速计算电路的软错误率。对ISCAS89及ISCAS85电路进行分析的实验结果表明：该方法与HSPICE仿真方法的平均偏差为4.12%,计算速度提升10000倍。该文方法可对大规模集成电路的软错误率进行快速分析。     

基于单次快拍的双基地MIMO雷达多目标角度估计方法

该文提出了一种双基地MIMO雷达体制下,利用单次快拍的回波数据进行多目标2维发射角(DOD)和2维接收角(DOA)联合估计的新方法。首先对等效接收阵数据的自相关矩阵进行发射分集平滑实现接收角(DOA)的估计,然后对等效发射阵数据的自相关矩阵进行接收分集平滑实现发射角(DOD)的估计,最后通过最大似然法完成两种角度的配对。该算法仅用一个时域快拍的数据实现了多目标回波的解相干,对发射和接收阵型有着广泛的适应性,同时为高速机动目标的角度测量提供了一种新的思路,仿真实验表明了该算法的有效性。