Nanoscopic Porous Iridium/Iridium Dioxide Superstructures (15 nm): Synthesis and Thermal Conversion by In Situ Transmission Electron Microscopy

Porous particle superstructures of about 15 nm diameter, consisting of ultrasmall nanoparticles of iridium and iridium dioxide, are prepared through the reduction of sodium hexachloridoiridate(+IV) with sodium citrate/sodium borohydride in water. The water-dispersible porous particles contain about 20 wt % poly(N-vinylpyrrolidone) (PVP), which was added for colloidal stabilization. High-resolution transmission electron microscopy confirms the presence of both iridium and iridium dioxide primary particles (1–2 nm) in each porous superstructure. The internal porosity (≈58 vol%) is demonstrated by electron tomography. In situ transmission electron microscopy up to 1000 °C under oxygen, nitrogen, argon/hydrogen (all at 1 bar), and vacuum shows that the porous particles undergo sintering and subsequent compaction upon heating, a process that starts at around 250 °C and is completed at around 800 °C. Finally, well-crystalline iridium dioxide is obtained under all four environments. The catalytic activity of the as-prepared porous superstructures in electrochemical water splitting (oxygen evolution reaction; OER) is reduced considerably upon heating owing to sintering of the pores and loss of internal surface area.     

JEM-2100PLUS透射电子显微镜操作方法与技巧及常见故障排除

以JEM-2100PLUS透射电子显微镜为例，介绍了电镜的基本结构、操作面板和成像原理。使用透射电子显微镜的最终目的就是要得到高质量的照片，结合透射电镜的操作步骤，总结了如何拍摄高质量的照片以及常见故障排除方法。     

Evolution of long-period stacking order (LPSO) in Mg97Zn1Gd2 cast alloys viewed by HAADF-STEM multi-scale electron tomography

We have studied three-dimensional (3D) structures and growth processes of 14H-type long-period stacking order (LPSO) formed in Mg₉₇Zn₁Gd₂ cast alloys by single tilt-axis electron tomography (ET) using high-angle annular dark-field scanning transmission electron microscopy. Evolution of the solute-enriched stacking faults (SFs) and the 14H LPSO by ageing were visualised in 3D with a high spatial resolution in multi-scale fields of views from a few nanometres to ~10 μm. Lateral growth of the solute-enriched SFs and the LPSO in the (0?0?0?1)_Mg plane is notable compared to the out-of-plane growth in the [0?0?0?1]_Mg direction. The 14H LPSO grows at the cost of decomposition of the (Mg, Zn)₃Gd-type precipitates, and accompany a change of in-plane edge angles from 30 to 60°. We have updated the Time–Temperature–Transformation diagram for precipitation in Mg₉₇Zn₁Gd₂ alloys: starting temperatures of both solute-enriched SFs and LPSO formation shifted to a shorter time side than those in the previous diagram.     

Effect of deprotonation on the magnetic exchange coupling constant of fluorene‐based verdazyl diradical: A computational study

The magnetic behavior of the fluorene bridged verdazyl diradicals has been studied theoretically in their neutral and deprotonated states. The deprotonation of C9‐H site of the fluorene ring opens a new coupling pathway, which changes the nature of magnetic coupling. The transmission spectra analysis reveals that the transmission through fluorine has also increased due to the opening of a new coupling path after deprotonation.     

Golf ball-assisted electrospray ionization of mass spectrometry for the determination of trace amino acids in complex samples

During the electrospray ionization (ESI) process, ions move through a heated capillary aperture to be detected on arrival at a mass analyzer. However, the ESI process creates an ion plume, which expands into an ion cloud with an area larger than that of the heated capillary aperture, significantly contributing to an ion loss of 50% due to coulombic repulsion. The use of DC and RF fields to focus ions from the ion source into the vacuum chamber has been proposed in the literature, but the improvement of ion transmission efficiency is limited. To improve ion transmission, in this study we propose a novel method using a home-made golf ball positioned between the ion source and the inlet of the mass analyzer to hydrodynamically focus the ions passing through the golf ball. The ion plume produced by the ESI process passes through the golf ball will reduce the size of the ion cloud then be focused and most of them flowed into the mass analyzer. Therefore, the sensitivity will be improved, the aim of this investigation is to study the enhancing of the signal using golf ball-assisted electrospray ionization liquid chromatography tandem mass spectrometry (LC-MS/MS) to determine 20 trace amino acids in complex samples, including tea, urine and serum. The results showed that the analytical performance of the determination of the 20 amino acids in tea, urine and serum samples using the home-made golf ball-assisted ESI source is better than that of a commercial ESI source. The signal intensities of the 20 amino acids were enhanced by factors of 2–2700, 11–2525, and 31–342680 in oolong tea, urine and serum analyses, respectively. The precision of the proposed method ranged from 1–9%, 0.4–9% and 0.4–8% at low, medium and high concentration levels of amino acids, respectively. The home-made golf ball-assisted ESI source effectively increased the signal intensity and enhanced the ion transmission efficiency and is also an easy, convenient and economical device. This technique can be applied to the analysis of trace compounds in complex matrices.     

FULLY SYMBOLIC GENERATION OF COMPLEX MULTIBODY MODELS*

Abstract

In this paper, a quasistatic finite element model of a spur gear pair is developed. A node-to-target contact formulation is given, where calculations of initial gaps are based upon the actual geometry of the gear flanks rather than upon a contact node and a facet or a line segment. By using a special contact search algorithm, profile modifications and mounting errors are easily incorporated in the analysis. The problem, which also includes friction, is solved by using a nonsmooth Newton method. The static transmission error can be calculated with accuracy with a relatively small number of nodes along the gear flanks. Several examples are given in order to demonstrate the model.     

Polarized light microscopy of the ferroelastic domains of YBa2Cu3O7−x

A short overview is given on recent polarized light microscopy studies of the orthorhombic ferroelastic domains and domain structures of YBa₂Cu₃O_7-x . The optical characteristics of large domains and lamellar domains with a high density of twin walls are pointed out, both for reflected and transmitted light. The polarizing microscope has allowed to observe the ferroelastic detwinning in situ and to determine the activation energy of the ferroelastic wall movements. The question of a potential ferroelectric phase transition is also discussed.     

h-BN型超晶格等离子体光子晶体能带特性研究

六方氮化硼(h-BN)晶格结构是一种类六方对称复式超晶格结构。具有h-BN晶格构型的光子晶体以其宽光子带隙特点受到国内外学者的广泛关注。本文利用不同尺度低压气体放电管与Al₂O₃介质棒周期性排列，构建了新型h-BN型超晶格等离子体光子晶体，实现其空间结构和等离子体参数的动态调控。利用微波透射谱对比研究了h-BN型超晶格与简单三角晶格等离子体光子晶体禁带位置、宽度和数目。分析了放电电流、介质棒阵列数对不同频段光子带隙的影响，以及电磁波入射角度对电磁传输特性的影响。结果表明：等离子体的引入不仅能够形成新的光子带隙，而且可以选择性地使部分禁带位置发生移动；相对于简单三角晶格，h-BN型超晶格等离子体光子晶体呈现出更多光子带隙；Al₂O₃介质棒阵列数对等离子体光子晶体禁带位置、宽度和数目均具有重要影响。电磁波入射角度变化越大，电磁传输特性差别越显著，透射谱相关性越差。本文所设计的新型h-BN型超晶格等离子体光子晶体为制作可调谐光子晶体提供了新的思路，在微波和太赫兹波控制领域具有潜在应用价值。     

浅析广州市花都区预防梅毒母婴传播的实施成效

目的了解花都区开展预防梅毒母婴传播阻断项目的实施成效,降低梅毒母婴传播率。方法对首次就诊的孕产妇进行梅毒筛查,对检出的梅毒阳性孕产妇进行规范治疗,并对其所生婴儿进行随访管理。结果 2012—2016年感染产妇孕期确诊率达71.18%,接受规范治疗率达53.02%,新生儿预防性治疗率75.8%,儿童3月龄梅毒检测率为50.86%,6月龄检测率42.55%。结论实施预防梅毒母婴传播项目,可以有效地阻断梅毒的母婴传播,降低梅毒母婴传播率,提高妇女儿童的健康水平。     

Azimuthal orientational correlations due to excluded volume epitaxy in growing anisotropic grains

The microstructure of anisotropically shaped grains can strongly influence a range of material properties, including transport, mechanical and electro-optical. A grain-structure-related phenomenon, known as excluded volume epitaxy (EVE), is reported in this study. EVE is a local, inter-grain orientational correlations effect, which results from a combination of continuous nucleation of anisotropic grains and impingement of growing grains. Due to EVE, anisotropically shaped grains have a tendency to be similarly aligned in a local neighbourhood, despite the absence of any forced global orientation in the sample. The effect has been repeatedly observed by the authors in block copolymers, as illustrated by a representative TEM image. Optical microscopy of anisotropically shaped non-polymeric crystals revealed the generality of this effect. The simulation study revealed a tendency for azimuthal, inter-grain orientational correlation and re-confirmed the experimental observation of EVE.