Microstructural investigation of the breakdown of the protective oxide scale on a 304 steel in the presence of oxygen and water vapour at 600 °C

This article focuses on the detailed microstructural investigation of the oxide scale formed on a 304 steel in the presence of oxygen and water vapour (40%) at 600 °C. The work has been carried out using a combination of microanalytical techniques including FIB, TEM, EDX and electron diffraction. The local breakdown of the initially protective oxide scale and the growth of island/crater oxide morphology are described. Special consideration is given to the influence of the microstructure of the steel and the oxide scale on the breakdown behaviour.     

Dispersion characterization in layered double hydroxide/Nylon 66 nanocomposites using FIB imaging

Layered double hydroxides (LDHs), a newly emerging 2D host material, consist of cationic brucite-like layers and exchangeable interlayer anions. In this work, the morphology and dispersion of LDH particles in LDH/Nylon 66 (salt) nanocomposites has been investigated using focused ion beam (FIB) techniques, transmission electron microscopy (TEM) and X-ray diffraction (XRD). The FIB images show that LDHs are present in the polymer phase dispersed to different degrees, with partial intercalation, exfoliation, and aggregation all being observed. The most even dispersion was achieved in nanocomposites with the lowest loading (0.5 wt % LDH). Residual tactoids and agglomerates were most common in the samples made with the highest concentration of LDHs studied here (5 wt %). The dispersion observed using FIB was consistent with TEM and XRD analysis, yet this technique had significant benefits in terms of time and simplicity over these “conventional” technologies. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

TEM and DFT investigation of CVD TiN/κ-Al2O3 multilayer coatings

This paper investigates the interfacial structure in hot-wall CVD TiN/κ-Al₂O₃ multilayer coatings using both HREM and DFT modeling. Two multilayers with different thicknesses of the TiN layers (50 and 600 nm) separating the κ-Al₂O₃ layers are analyzed. The general microstructure of the two multilayers is relatively similar. The TiN layer in the thicker TiN/κ-Al₂O₃ coating is thick enough to be several TiN grains high. This means that epitaxial columns, which are often found in the thinner TiN/κ-Al₂O₃ coatings, are not present. However, the orientation relationships at the TiN/κ-Al₂O₃ interfaces are the same in both multilayers. The HREM investigations show that κ-Al₂O₃ (001) planes can grow directly on flat (111) TiN faces, without any other phases or detectable amounts of impurities, such as sulphur, present. Where the TiN layers are more curved, γ-Al₂O₃ can be grown, at least partly stabilized by the cube-on-cube orientation relationship between γ-Al₂O₃ and the underlying TiN. The DFT calculations show very similar adsorption strengths for an O monolayer positioned on Ti-terminated TiC(111) and TiN(111) surfaces, with preferred adsorption in the fcc site. O adsorption on N-terminated TiN(111) is much weaker, with preferred adsorption in the top site. Calculated elastic-energy contributions yield a higher stability for κ-Al₂O₃ on TiN(111) than on TiC(111) and a higher stability for κ-Al₂O₃ than for α-Al₂O₃ on both TiC and TiN. This indicates that the observed higher stability of κ-Al₂O₃ on TiC(111) than on TiN(111) is not due to the lattice mismatch, while the preferred epitaxial growth of κ-Al₂O₃ over α-Al₂O₃ can be partly attributed to the mismatch.     

Characterisation and behaviour of Ti/TiO2/noble metal anodes

The morphology, composition and the electrical and electrochemical behaviour of the anodic microporous layer, prepared by the galvanostatic anodisation of Ti after sparking, followed by galvanostatic deposition of Pt or Ir have been investigated. These electrodes are proposed to function as dimensionally stable anodes (DSAs). For Ti/TiO₂/Pt electrodes, Pt is deposited within some of the micropores of the oxide film. In contrast, for Ti/TiO₂/Ir, the metal is deposited preferentially on the top surface. This difference is thought to result from the position of the metal deposition potential with respect to the flat band potential of n-TiO₂. Optical imaging of both types of DSA suggests that only a few sites on the surface are responsible for electron exchange at the DSA-electrolyte interface. C-AFM measurements of Ti/TiO₂/Pt samples subjected to long-term anodic polarisation, suggest that the Ti-noble metal contact is progressively insulated by thickening of the TiO₂ barrier layer, promoting passivation of the DSA. For Ir coated anodes, catalytic activity is directly related to the presence of Ir and to the stability of the catalytic oxide layer. Under Cu electrowinning conditions, the electrochemically formed hydrated Ir oxide was found to be catalytically less stable, than the iridium oxide film subjected to a heat treatment.     

Microstructural Investigation of Protective and Non-Protective Oxides on 11% Chromium Steel

FIB, SEM and STEM/EDX were used to investigate X20 stainless-steel samples exposed to dry O₂, or O₂ containing 40% H₂O, with a flow velocity of 0.5 cm/s or 5 cm/s, for 168 hr or 336 hr at 600°C. Thin protective Cr-rich (Cr,Fe)₂O₃ was maintained on the samples exposed to dry O₂, even after 336 hr, and on the sample exposed to O₂/H₂O mixture with the low-flow velocity (0.5 cm/s) for 168 hr. The oxide scale formed in the latter environment contained less Cr, due to Cr loss through CrO₂(OH)₂ evaporation. Breakaway oxidation occurred on the samples exposed in high-gas-flow velocity for shorter time (168 hr) or in low-gas-flow velocity (0.5 cm/s) for longer time (336 hr). The breakaway scales featured a two-layered structure: an outward-growing oxide “island” consisting of almost pure hematite (α-Fe₂O₃), and an inward-growing oxide “crater” consisting of (Cr,Fe)₃O₄. The transition from a thin protective (Cr,Fe)₂O₃ scale to a non-protective thick scale on this martensitic/ferritic steel originated locally and was followed by rapid oxide growth, resulting in a thick scale that covered the whole sample surface.     

Investigation into the evolution of corrosion product layer (CPL) of 1018 C-steel exposed to multiphase environment using FIB and EIS techniques

This communication reports into the effects of flow, fluid composition and the effectiveness of imidazoline inhibitors on the evolution and distribution of corrosion products on 1018 C-steel exposed to CO₂ corrosion. Focused ion beam technique was used to measure the thickness of the corrosion product layer (CPL), in contrast to the conventional techniques used to observe the cross-section of specimens. Morphological analysis using scanning electron microscopy revealed topographical variations on the surface with the change in the multiphase environment. The CPL was found to be more porous in nature with the presence of oil in the multiphase environment. Electrochemical impedance spectroscopy was also used in the present study to measure the corrosion rates and was subsequently correlated to the CPL evolution for 1018 C-steel in multiphase environment.     

Effect of micro-electrode geometry on NO2 gas-sensing characteristics of one-dimensional tin dioxide nanostructure microsensors

Electrodes with micro-gaps are fabricated by using dc-sputtering and FIB techniques. SnO₂ nanowires are deposited on the micro-gap (1-30 μm) by suspension dropping method to fabricate a micro-gas sensor. The sensing ability of various SnO₂ micro-gap sensors is measured. A comparison between sensors reveals that the short-gap electrode has numerous advantages in terms of reliability, high sensitivity and detection of low concentrations of NO₂, while the large-gap electrode is relatively sensitive for high concentrations. Conductance measurements are carried out at different surface temperatures and NO₂ concentrations in order to investigate the effects that the gap size has on the overall sensor conductance. The results suggest that the interface between the electrode and sensitive layer has a very important role for the sensing mechanism of tin dioxide gas sensors.     

exFAT文件系统的优化模型

针对exFAT文件系统查询FAT表时会读取大量无效数据的问题,提出一种阻止无效数据读取,加快文件查询速度,且代价较小的优化模型。优化模型在flash中建立簇链表,顺序存储已读文件的FAT表信息,在系统RAM中建立文件信息块,保留该次运行常用文件的簇链表入口地址。以此快速查询文件FAT表信息。实验结果表明,FAT表离散度越大,速度和效率的优化效果越明显。     

Imaging and analysis of 3-D structure using a dual beam FIB

The application of focused ion beam instrumentation in the generation of three-dimensional microstructural data is described. The methodologies used to acquire and manipulate this data are explained, and the technique is illustrated by a number of examples from the material sciences. The limitations of this method, and practical pointers to the generation of meaningful data, are also discussed.     

宽带多协议标记交换（MPLS）网络的原理及关键技术

多协议标记交换（MPLS）技术将网络层路由功能和数据链路层交换功能相结合,充分利用第三层和第二层功能,被认为是下一代Internet的基础技术,本文介绍了其基本原理和关键技术。