EDS X-Ray Investigation of Interdiffusion in Au–Ni Micro- and Nanolayers

The interdiffusion process in thin and thick (500nm–60µm) Au–Ni layers deposited on different substrates is studied using the EDS technique. In-depth X-ray analysis based on the Pouchou and Pichoir method is applied for obtaining the concentration profiles in nanometre scale multi-layers. A theoretical analysis using the Darken method is employed for modelling interdiffusion in the Au–Ni system. Computer simulations, where intrinsic diffusivities of the Au and Ni are functions of composition, are presented and compared with experimental results.     

Uranium association with corroding carbon steel surfaces

We investigated the association of uranium with clean and corroded surfaces of 1010 carbon steel. Studying steel contaminated by uranium species will have an important effect on the development of methods used to clean radioactively contaminated metal waste. X‐ray photoelectron spectroscopy, synchrotron infrared microspectroscopy and laboratory‐based Fourier transform infrared analysis of steel surfaces exposed to uranyl nitrate showed the presence of crystallized hydrated uranyl oxides, uranyl hydroxides, iron oxyhydroxides and iron oxides. In general, heavily corroded areas physically shield the uranium species, which tended to associate spatially with hydroxyl groups and lepidocrocite. Lightly corroded areas contained uranium species with stronger axial U–O bonding. Infrared spectroscopy, Rutherford backscattering spectroscopy and energy‐dispersive spectroscopy mapping analysis revealed that the uranium species are well distributed within the upper micron of the thick corrosion layer and associated more with areas of high hydroxide content. Parameters such as the concentration of uranyl nitrate solution used to expose the carbon steel coupons, the method of contamination (dipped or sprayed with dilute uranyl nitrate solution) and the degree of corrosion (accelerated corrosion before and/or after contamination) played significant roles in the distribution and nature of the uranyl hydroxide/iron oxyhydroxide corrosion products found on the surface of all coupons. These factors must be considered in the development and optimization of decontamination processes for metal waste. Copyright © 2003 John Wiley & Sons, Ltd.     

Design and Application of a Set of Vitreous Standards for EDS-SEM Microanalysis of Melting Shop Slags

Non-metallic inclusions in steel are formed due to interactions between liquid steel and its environment in the melting shop (refractories and slags). Particles not trapped in the slag remain in the cast steel, impairing steel properties in service. Inclusion composition varies and certified standards covering the whole compositional range are unavailable.The present study describes the preparation of a set of homogeneous, glassy and crystalline standards with a wide compositional range for use in analysing non-metallic steel inclusions. For this, materials were designed based on knowledge of the compositional range of interest in the Al₂O₃–SiO₂–CaO–MgO–CaF₂ system, which is the matrix of the most frequent steel inclusions. The composition and microstructural homogeneity of the reference materials was verified.     

Analysis of polished polycrystalline diamond using dual beam focused ion beam microscopy

This paper presents a study on polycrystalline diamond (PCD) polished by dynamic friction polishing (DFP) with the aid of advanced dual beam FIB (focused ion beam) microscopy. After disclosing a variety of wear tracks by DFP using electron imaging in combination with the ion channelling effect, a dual beam FIB was successfully employed at wear track sites to specifically create both the large cross-sectional specimen for microanalysis and thin foil for nanoanalysis. The study concluded that the polished PCD subsurface was free from microscale cracking. However, the attached debris layer on the top surface contained metal oxides and non-diamond carbon phase with inhomogeneous distributions of C, Fe, Cr, Ni, Si and O across the layer. An attached layer directly above a diamond grain was composed of essentially amorphous carbon, suggesting that a direct phase transformation from diamond crystalline to amorphous occurred during DFP.     

The secondary X-ray fluorescence and absorption near the interface of multi-material: Case of EDS microanalysis

A simple model is proposed to take into account secondary X-ray fluorescence and absorption effects near the interface. This model is based on the investigation of the shape change of the first derivative equation that can fit the sigmoidal EDS profile obtained when a high vacuum electron beam passes through the interface of two adjacent materials. The contribution of the photoelectric absorption of primary X-rays (characteristic and Bremsstrahlung) and the secondary fluorescence on the degradation of the X-ray spatial resolution can be easily quantified. The close agreement between the simulated (Monte Carlo simulation using the Casino software) and the experimental data serves to assess the reliability of this developed model.     

单元和多元取代纳米氢氧化镍晶相及其结构稳定性研究

以硝酸镍为镍源,硫酸钴、硫酸铜、硫酸铝为掺杂原料,采用超声波辅助沉淀法分别制备了单元和多元取代纳米氢氧化镍。用X射线衍射（XRD）、傅里叶变换红外光谱（FTIR）、激光粒度仪（PSD）及电子显微镜（TEM、SEM）对样品晶相结构、形貌、粒度分布等进行了表征,研究了单元或多元取代对产物晶相及其结构稳定性的影响。结果表明,样品均为纳米级Ni（OH）₂,随着掺杂元素种类的增多,其一次粒子变得细小,团聚加重,二次粒子粒径增大。样品中α-Ni（OH）₂比例随取代元素增多而增大。相对于Co单元和Co/Cu双元取代,Co/Cu/Al三元取代的样品其晶相结构更稳定,在碱液中浸泡3周后仍为纯α-Ni（OH）₂。在相同掺杂比例下,Cu取代比Co取代更有利于α-Ni（OH）₂的生成,但Co取代的样品结构稳定性优于Cu取代的样品。     

ESEM-EDS: In vivo characterization of the Ni hyperaccumulator Noccaea caerulescens

Environmental scanning electron microscopy (ESEM) permits to analyze samples in their native-hydrated state, allowing a broad spectrum of biological applications. In this study, ESEM equipped with energy dispersive X-ray spectrometer (EDS) was used as a fast method to analyze tissue morphology and to investigate metal distribution in the Ni hyperaccumulator Noccaea caerulescens, an established model to study the adaptation of plants to metalliferous soils. The low vacuum and wet mode operative conditions required the proper choice of experimental parameters both for morphological and compositional characterization of plant tissues. The calibration strategy for semi-quantitative analysis involved the use of Ni fortified agar as standard and signal normalization respect to endogenous carbon, chosen as internal standard. The obtained results are in accordance with present literature, showing a preferential Ni distribution in the epidermal cells respect to near the stomata for leaves and in the cotyledon epidermidis respect to cotyledon parenchyma area for seeds. Thanks to the absence of any time consuming sample treatment steps, ESEM-EDS technique can be proposed as valid strategy for in vivo high-throughput analysis of plant tissues and for a rapid screening and identification of other hyperaccumulator plants in a selected contaminated area.     

给定割点数的简单连通图的最小EDS极图

图的EDS(偏心距离和)是图的一个类似于Wiener指数的另一个重要指数,近年来受到广泛的关注.2012年H.B.Hua等在Discrete Appl.Math.中的一篇关于图的EDS极图的论文中提出一个问题:哪些图是具有k个割点及最大或最小EDS的极图?通过研究图的EDS确定了给定割点数为k的简单连通图的最小EDS极图.     

Influence of the Oxide Content in the Catalytic Power of Raney Nickel in Hydrogen Generation

The influence of oxides in the hydrogen evolution on Raney nickel electrocatalysts was characterized by electrochemical impedance measurements. In addition, these materials show competitive overpotentials for hydrogen evolution with a modified Watts bath as a binder for the Raney nickel. The optimum result was ?190?mV of overpotential at 100?mA?cm^?2. Oxygen in the Raney Ni catalyst affects its electroactivity toward hydrogen evolution. The source of oxygen is related to the presence of chloride ions in the modified Watts bath. A Watts bath binds Raney Ni particles to the surface of the catalysts and chloride regulates the oxygen content in the nickel binder during electrodeposition. High oxygen content increases the hydrogen evolution overpotential of the electrode. The electroactivity of the synthesized porous coatings was evaluated by polarization curves and impedance plots. In addition, surface characterization by X-ray diffraction, field emission–scanning electron microscopy equipped with energy-dispersive analysis, and X-ray photoelectron spectroscopy is reported.     

采用FTIR和电子能谱EDS指纹图谱直观比对鉴定右归丸济生肾气丸

结合FTIR和电子能谱EDS指纹图谱,鉴别了两种组成相近的中药复方右归丸和济生肾气丸.测定右归丸和济生肾气丸样品氯仿提取物的红外指纹图谱,依据W检验理论判别方法精细建立两种中药复方红外指纹图谱的特征吸收峰组,确定了各个特征吸收峰相对应的特征分子基团和药物成分组成.同时测量两种中药复方原药粉末样品的EDS指纹图谱.根据两...