An electron microscopy three‐dimensional characterization of titania nanotubes

To characterize complex, three‐dimensional nanostructures, modern microscopy techniques are needed, such as electron tomography and focused ion beam (FIB) sectioning. The aim of this study was to apply these two techniques to characterize TiO₂ nanotubes in terms of their size, shape, volume, porosity, geometric surface area, and specific surface area (SSA). For these experiments, titania nanotubes were fabricated by means of the electrochemical oxidation of titanium at a voltage of 20 V for 2 hr followed by heat treatment at 450°C for 3 hr to change the amorphous structure into a crystalline anatase structure. The quantitative data obtained from the FIB and electron tomography reconstructions show a high similarity in porosity and some differences in SSA. These might be the result of differences in resolution between the two reconstruction techniques.     

A model of splats deposition state and wear resistance of WC-10Co4Cr coating

In this research both low temperature high velocity oxygen-fuel flame (LT-HVOF) and high velocity oxygen-fuel flame (HVOF) techniques were employed to prepare WC-10Co4Cr splats and coatings. In situ cutting of WC-10Co-4Cr splats was carried out with focused ion beam (FIB), and a model was proposed to describe how the wear resistance of WC-10Co4Cr coatings was correlated with its residual stress state and the splats deposition state. It was observed that in LT-HVOF spraying process, WC-10Co4Cr splats were slightly melted showing "hill" shape, while in HVOF spraying process, the splats were half melted having the appearance of "concavity". The residual stress of WC-10Co4Cr coatings is determined by the size, melting state, flight speed and temperature gradient of splats. In this paper, the quantitative function formula involving heating temperature and the flight speed of the powder is put forward for the first time to predict the wear resistance of the WC-10Co4Cr coatings. This will provide a theoretical basis for engineering practice and an effective way to save costs.     

Investigating material removal rate and surface roughness using multi-objective optimization for focused ion beam (FIB) micro-milling of cemented carbide

Cemented carbide has been investigated as a useful material for the fabrication of micro devices. Focused ion beam (FIB) micro-milling has been found to be one of the most appropriate methods for the fabrication of micro devices. The experimental FIB micro-milling on cemented carbide have been conducted according to the L₁₆ orthogonal array of Taguchi technique. Beam current, extraction voltage, angle of beam incidence, dwell time and percentage overlap between beam diameters have been considered as process variables of FIB micro-milling in experimental design. Material removal rate (MRR) and surface roughness have been determined experimentally for FIB micro-milling of cemented carbide and beam current has been identified as the most significant parameter. The minimum surface roughness of 5.6 nm has been reported on cemented carbide, which is not a usual practice to achieve on such polycrystalline material, and hence it may be considered as a significant research contribution. Maximum MRR of 0.4836 μm³/s has been reported. Moreover, genetic algorithm toolbox of MATLAB has been utilized for multi-objective optimization between MRR and surface roughness. The corresponding optimum values of MRR and surface roughness for multi-objective optimization have been represented by pareto optimum solution generated by genetic algorithm. The research work presented in this paper determines the setting of process parameters of FIB micro-milling for achieving a specific combination of MRR and surface roughness on cemented carbide.     

Reconstructing the microstructure of polyimide–silicalite mixed‐matrix membranes and their particle connectivity using FIB‐SEM tomography

Properties of a composite material made of a continuous matrix and particles often depend on microscopic details, such as contacts between particles. Focusing on processing raw focused‐ion beam scanning electron microscope (FIB‐SEM) tomography data, we reconstructed three mixed‐matrix membrane samples made of 6FDA‐ODA polyimide and silicalite‐1 particles. In the first step of image processing, backscattered electron (BSE) and secondary electron (SE) signals were mixed in a ratio that was expected to obtain a segmented 3D image with a realistic volume fraction of silicalite‐1. Second, after spatial alignment of the stacked FIB‐SEM data, the 3D image was smoothed using adaptive median and anisotropic nonlinear diffusion filters. Third, the image was segmented using the power watershed method coupled with a seeding algorithm based on geodesic reconstruction from the markers. If the resulting volume fraction did not match the target value quantified by chemical analysis of the sample, the BSE and SE signals were mixed in another ratio and the procedure was repeated until the target volume fraction was achieved. Otherwise, the segmented 3D image (replica) was accepted and its microstructure was thoroughly characterized with special attention paid to connectivity of the silicalite phase. In terms of the phase connectivity, Monte Carlo simulations based on the pure‐phase permeability values enabled us to calculate the effective permeability tensor, the main diagonal elements of which were compared with the experimental permeability. In line with the hypothesis proposed in our recent paper (?apek, P. et al. (2014) Comput. Mater. Sci. 89 , 142–156), the results confirmed that the existence of particle clusters was a key microstructural feature determining effective permeability.     

Advanced FIB sample preparation techniques for high resolution TEM investigations of HEMT structures

In this paper advanced sample preparation techniques based on focused ion beam (FIB) optimized for TEM investigation of high electron mobility transistor (HEMT) structures are presented. It is shown that the usage of an innovative in-situ lift-out method combined with X2 window and backside milling techniques as well as live thickness control and end point detection can significantly improve the quality of electron transparent samples required for high resolution TEM investigations. This advanced preparation flow is evaluated and demonstrated at GaN HEMT structures for atomic resolution TEM investigation.     

Efficient and flexible Focused Ion Beam micromachining of Solid Immersion Lenses in various bulk semiconductor materials – An adaptive calibration algorithm

Focused Ion Beam (FIB) micromachining of Solid Immersion Lenses (SILs) in substrate material offers optical analysis solutions for current and future technologies without the limitations of external SIL systems. This work presents an efficient single iteration calibration algorithm. This algorithm enables the implementation of FIB created SILs using a variety of substrate materials, process chemistries and most importantly different SIL shapes to match sample thicknesses. The successful application on silicon and silicon carbide is presented by creating a 50 μm wide refractive lens segment with a radius of curvature of 60 μm. Laser scanning microscope images of a silicon sample demonstrate the optical benefit with a measured resolution of 274 nm.     

Non‐destructive detection of corrosion applied to steel and galvanized steel coated with organic paints by the pulsed phase thermography

Organic coatings in the automobile industry have to resist corrosion and mechanical damage from stone chipping. Currently, no tool is established in industrial non‐destructive applications for analyzing the damage of stone‐impacts and the following corrosion after accelerated corrosion tests. Measurement methods such as the scanning Kelvin probe can analyze the corrosion progress in a detailed manner, but with a long measurement time. The pulsed phase thermography (PPT) is a non‐destructive tool to analyze inhomogeneities and defects in materials, with a huge field of applications existing. The present work shows advances in using the PPT to detect propagation of corrosion under coatings. Physical principles of the mechanism of the corrosion detection under coatings are described. Results of measurements of organic coatings on carbon steel as well as of organic coated galvanized steel show the corrosion propagation. Influencing factors to the measurement such as the thickness of the coatings are investigated, but no significant effect on the quality of the analysis was found. The corrosion progress can be monitored by the PPT fast and reliably. The achieved results correlate with the theoretical basis and the test results after surface characterization and destructive analysis of samples.     

Micro machining for control of wettability with surface topography

A micro fabrication is presented to manufacture hydrophobic surfaces with micro-scale structures. Hydrophobicity is controlled with the shape and the alignment of micro pillars in the structure. The structures are manufactured in large areas at high production rates in the following processes: (1) the structure is fabricated on a tool by focused ion beam sputtering; (2) the reverse structure is formed on a metal plate by incremental stamping using the structured tool; and (3) the structure is transferred onto plastic plates by molding. A consecutive stamping is also proposed to fabricate several structures on a surface accurately with a structured tool, in which the moving pitch of the structured tool is numerically controlled. The effect of the surface topography on hydrophobicity is discussed with measuring contact angles on the structured surfaces in the water droplet tests. Hydrophobicity on the plastic plate is associated with the solid fraction on the structured surface based on the Cassie–Baxter model. A larger contact angle is observed for a smaller solid fraction of the surface.     

冷喷涂单颗粒铜在铝基体上的显微结构研究

采用冷喷涂法在铝(Al)基体上沉积单颗粒铜(Cu),利用聚焦离子束/电子束(FIB/SEM)系统精确定位并原位制备了完整单个颗粒Cu沉积在Al基体上的透射样品,分析其显微结构及形成原因。实验结果表明,撞击过程中温度与应力分布不均匀,导致沉积Cu颗粒不均匀形变。Cu/Al界面受影响较大:颗粒动能转化为形变能和热能,打破了界面处氧化膜,使界面附近温度迅速升高,发生动态再结晶,生成金属间化合物Cu_9Al_4;Cu颗粒内距界面越远的区域,受温度和应力的影响越小,其变形主要是通过晶体内位错增殖和移动;沉积颗粒顶部,远离Cu/Al界面,几乎不受应力和温度影响,保持原始显微结构。