Liquid hydridosilane precursor prepared from cyclopentasilane via sonication at low temperatures without the action of light

We report on a liquid hydridosilane precursor ink prepared via the ultrasonically induced ring-opening polymerisation of cyclopentasilane (Si₅H₁₀) without irradiation by ultraviolet light. The sonication is carried out in N₂ atmosphere at temperatures between 20 and 75 °C. We use size exclusion chromatography (SEC) to show polymer growth and estimate molecular mass with increasing sonication time. In combination with UV–vis transmission measurements, further SEC analysis is used to compare solutions subjected to either purely thermal or ultrasonic treatment at the same process temperature and for the same duration. Our findings provide strong evidence showing that the initiation of the polymerisation is sonocatalytic in nature and not thermic due to the macroscopic temperature of the solution. The liquid precursor is used to produce homogeneous hydrogenated amorphous silicon (a-Si:H) thin films via spin coating and pyrolytic conversion. The optoelectronic properties of the films are subsequently improved by hydrogen radical treatment. Fourier transform infrared spectroscopy (FTIR) is used to determine a compact film morphology and electrical conductivity measurements show that the layers attain a light-to-dark photosensitivity ratio of 2 × 10³ making them suitable for application in optoelectronic devices.     

A discussion on mass resolution in secondary ion mass spectrometry

Mass resolution is a very important parameter for mass spectrometry. It is necessary to compare the mass resolution between the newly developed TOF-SIMS and the conventionally high-performance magnetic SIMS. However, the definitions of mass resolution for these two types of instruments are quite different. Whether it is possible to compare mass resolution and how to do such comparison is a challenge. This problem was raised officially during the 2012 ISO/TC 201 meeting at Tampa, Florida, the United States and the long-term cooperation with ISO started afterwards. The definition of mass resolution is one of the most important and fundamental problems for mass spectrometry and should attract significant attention. Here, some detail discussions on mass resolution as well as the related experimental studies in the past few years, including the collaborations with ISO/TC 201/SC6 and SC1 are summarized. This summary covers the common problem for almost all the current existing and still used definitions of mass resolution. A reasonable new definition for mass resolution considering the peak shape or resolution function has been proposed, which has also been confirmed by using experimental studies of the mass resolution comparison between TOF and magnetic SIMS. This study lays a foundation for the future mass resolution comparisons between different mass spectrometry.     

Heteronuclear Cross‐Relaxation Effects in the NMR Spectroscopy of Hyperpolarized Targets

Dissolution dynamic nuclear polarization (DNP) enables high‐sensitivity solution‐phase NMR experiments on long‐lived nuclear spin species such as ¹⁵N and ¹³C. This report explores certain features arising in solution‐state ¹H NMR upon polarizing low‐γ nuclear species. Following solid‐state hyperpolarization of both ¹³C and ¹H, solution‐phase ¹H NMR experiments on dissolved samples revealed transient effects, whereby peaks arising from protons bonded to the naturally occurring ¹³C nuclei appeared larger than the typically dominant ¹²C‐bonded ¹H resonances. This enhancement of the satellite peaks was examined in detail with respect to a variety of mechanisms that could potentially explain this observation. Both two‐ and three‐spin phenomena active in the solid state could lead to this kind of effect; still, experimental observations revealed that the enhancement originates from ¹³C→¹H polarization‐transfer processes active in the liquid state. Kinetic equations based on modified heteronuclear cross‐relaxation models were examined, and found to well describe the distinct patterns of growth and decay shown by the ¹³C‐bound ¹H NMR satellite resonances. The dynamics of these novel cross‐relaxation phenomena were determined, and their potential usefulness as tools for investigating hyperpolarized ensembles and for obtaining enhanced‐sensitivity ¹H NMR traces was explored.     

Ku波段扩展互作用速调管设计

 微波电真空器件随着频率的升高,不但聚焦系统难以实现,而且其输出增益和带宽都受到很大的限制,要解决该问题,建议采用扩展互作用速调管,采用分布作用谐振腔技术来扩展其工作带宽和提高增益。利用CST和粒子模拟(PIC)3维软件对其工作在Ku波段扩展互作用速调管进行了设计和仿真,在工作电压30 kV、束流8.5 A的条件下,聚焦系统采用幅值为0.48 T的周期反转永磁聚焦,在输入功率为5.1 W时,得到效率为23%,3 dB带宽为306 MHz,频带内最大增益为39 dB,其峰值功率为58 kW的微波输出。     

同位镀铋膜电极测定爆米花中的痕量铅

采用同位镀铋膜法修饰铂电极,用差分脉冲溶出伏安法对爆米花中痕置铅进行了测定,并优化了实验条件.在优化的实验条件下,分别对2.0×10<'8>-6.0×10<'-7>mol/L和6.0×10<'-7>-1.0×10<'-4>mol/L的pb<'2+>进行了测定,Pb<'2+>溶出峰电流与Pb<'2+>浓度呈良好的线性关系...     

圆柱装药在偏心定向起爆时水中近场压力特性

对UHL-5装药在侧向9点偏心定向起爆和几何中心点起爆时的水下爆炸近场峰值压力分布特性进行实验研究和数值模拟,得到2种起爆条件下不同距离与方位角测点处冲击波峰值压力和侧向9点起爆时的定向增益区域.结果表明,对于5 kg圆柱形UHL-5装药,采用侧向9点偏心定向起爆方式时,在爆距750 mm、方位角90°范围内的流场区域...     

径向直线槽端面密封空化特性数值模拟

基于质量守恒边界条件,建立了径向直线槽端面密封空化特性的数值模型.控制方程为考虑惯性的定常不可压缩Reynolds方程,利用有限控制体积法对其进行离散,采用分块加权方法计算膜厚突变处流量,迭代方法为Gauss-Siedel松弛迭代,并对空化特性影响因素进行了分析.结果表明：不同工况下,油膜破裂位置均在膜厚突然增大处,密封坝阻碍空化的产生;空穴区域随着转速的增大而增大,随着槽深的增大而减小;空化区域在径向由静压决定,周向由动压决定,二者对空化的影响相互独立.     

Compromising Science by Ignorant Instrument Calibration—Need to Revisit Half a Century of Published XPS Data

X‐ray photoelectron spectroscopy (XPS) is an indispensable technique in modern materials science for the determination of chemical bonding as evidenced by more than 10 000 XPS papers published annually. A literature survey reveals that in the vast majority of cases an incorrect referencing of the binding energy scale is used, neglecting warnings that have been formulated from the early days of the technique. Consequences for the data reliability are disastrous and decades of XPS work require revisiting. The purpose of this Viewpoint is to highlight the existing problems, review the criticism and suggest ways forward.     

Wavelet transforms in separation science for denoising and peak overlap detection

Wavelet transform is a versatile time‐frequency analysis technique, which allows localization of useful signals in time or space and separates them from noise. The detector output from any analytical instrument is mathematically equivalent to a digital image. Signals obtained in chemical separations that vary in time (e.g., high‐performance liquid chromatography) or space (e.g., planar chromatography) are amenable to wavelet analysis. This article gives an overview of wavelet analysis, and graphically explains all the relevant concepts. Continuous wavelet transform and discrete wavelet transform concepts are pictorially explained along with their chromatographic applications. An example is shown for qualitative peak overlap detection in a noisy chromatogram using continuous wavelet transform. The concept of signal decomposition, denoising, and then signal reconstruction is graphically discussed for discrete wavelet transform. All the digital filters in chromatographic instruments used today potentially broaden and distort narrow peaks. Finally, a low signal‐to‐noise ratio chromatogram is denoised using the procedure. Significant gains (>tenfold) in signal‐to‐noise ratio are shown with wavelet analysis. Peaks that were not initially visible were recovered with good accuracy. Since discrete wavelet transform denoising analysis applies to any detector used in separation science, researchers should strongly consider using wavelets for their research.