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The objective of the present work was to study the impact of Focused Ion Beam (FIB) machining parameters on the thickness of the damaged layer within a thin film PZT. Therefore, different Ga+- ion doses and ion energies were applied to a standard PZT film (80/20 lead zirconium titanate) under two beam incidence angles (90° and 1°). The thicknesses of the corresponding Ga+-implanted layers were then determined by cross-sectional TEM in combination with energy dispersive spectroscopic (EDS) line-scans and correlated with polarisation hysteresis loops. The results show a decrease of Ga+-implanted layer thickness with decreasing inclination angle, whereas ion energy and ion dose could be correlated with gallium concentration in the implanted layers.. Under the most unfavorable conditions the depth of the affected zone was 26 nm, it was only 2 nm for the most favorable conditions.
Silica nanowires spanning 10 μm-deep trenches are fabricated from different types of silsesquioxane-based precursors by direct e-beam patterning on silicon followed by release through deep reactive ion etching. Nanowire aspect ratios as large as 150 are achieved with a critical dimension of about 50 nm and nearly rectangular cross-sections. In situ bending tests are carried out inside a scanning electron microscope, where the etch depth of 10 mm provides sufficient space for deformation. Silica NWs are indeed observed to exhibit superplastic behavior without fracture with deflections reaching the full etch depth, about two orders of magnitude larger than the nanowire thickness. A large-deformation elastic bending model is utilized for predicting the deviation from the elastic behavior. The results of forty different tests indicate a critical stress level of 0.1–0.4 GPa for the onset of plasticity. The study hints at the possibility of fabricating silica nanowires in a monolithic Fashion through direct e-beam patterning of silsesquioxane-based resins. The fabrication technology is compatible with semiconductor manufacturing and provides silica nanowires with a very good structural integrity.
The quantitative nanomechanical characterization of soft materials using the nanoindentation technique requires further improvements in the performances of instruments, including their force Resolution in particular. A micro-machined silicon nanoforce transducer based upon electrostatic comb drives featuring the force and depth resolutions down to 1 nN and 0.2 nm, respectively, is described.
At the end of theMEMStransducer’s main shaft, a pyramidal tip is fabricated using a focused ion beam facility. A proof-of-principle setup with this MEMS nanoindenter has been established to measure the mechanical properties of soft polydimethylsiloxane. First measurement results demonstrate that the prototype measurement system is able to quantitatively characterize soft materials with elastic moduli down to a few MPa.
A combined methodical approach is tested with respect to the characterization of the inner structure of porous TiO2 layers as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area of the pore network. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). Size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted.
Thin Sol-Gel Alumina Coating as Protection of a 9% Cr Steel Against Flue Gas Corrosion at 650 °C
(2018)
Samples of sol-gel alumina coated and uncoated P92 steel were exposed to flue gas at 650 °C for 300 h. As result of this treatment a 50 µm thick bi-layered oxide scale had formed on the surface of the uncoated sample. Below the scale a 40 µm thick inner oxidation zone was detected. In contrast, the porous, micron thick alumina coating enabled the formation of a chromium oxide scale with a thickness of some nanometers at the interface between steel substrate and coating. In this case high temperature corrosion of the steel was prevented so far.
Technically relevant P92 steel (9% Cr) was coated with a micron-thick porous alumina layer prepared by sol-gel technique and treated with flue gas (60 CO2-30 H2O-2 O2-1 SO2-7 N2 (mole fraction in %)) at 650 ° to mimic an oxyfuelcombustion process. Local defects in the coating were marked using focused ion beam (FIB) technique and were inspected after exposition to hot flue gas atmosphere at 300, 800, and 1300 h, respectively. Local defects like agglomerated alumina sol particles tend to spall off from the coating uncovering the underlying dense chromia scale. Re-coating was found to restore the protection ability from oxidation when repeatedly treated with hot flue gas. Cracks and voids did not promote the local oxidation due to the formation of crystalline Mn/S/O species within and on top of the coating. The protective character of the steel-coating system is a result of (i) the fast formation of a dense chromia scale at the surface of sol-gel alumina-coated P92 steel bars in combination with (ii) the porous alumina coating acting as diffusion barrier, but also as diffusion partner in addition with (iii) fast Mn outward diffusion capturing the S species from flue gas.
Metal sulfide grain boundary precipitates of a ferrous model alloy with 13 wt.% chromium formed at 650°C under a gas atmosphere containing 0.5% SO2 and 99.5% Ar were investigated after ageing for 3 h, 6 h, and 12 h. The precipitates formed along grain boundaries were identified as Cr5S6 using energy-dispersive x-ray spectroscopy in transmission electron microscopy and electron backscatter diffraction analysis. Serial focused ion beam slicing was conducted followed by three-dimensional reconstruction to determine the number, size, and penetration depth of the precipitates evolved at the different time steps. There was a linear increase in the number of precipitates with time, while their average size increased only for the initial aging time but became constant after 6 h. Based on these results, a model for grain boundary sulfidation of ferritic alloys is discussed.
Nanoscale building blocks impart added functionalities to microelectromechanical systems (MEMS). The integration of silicon nanowires with MEMS-based sensors leading to miniaturization with improved sensitivity and higher noise immunity is one example highlighting the advantages of this multiscale approach. The accelerated pace of research in this area gives rise to an urgent need for batch-compatible solutions for scaling to nano. To address this challenge, a monolithic fabrication approach of silicon nanowires with 10-lm-thick silicon-on-insulator (SOI) MEMS is developed in this work. A two-step Si etching approach is adopted, where the first step creates a shallow surface protrusion and the second step releases it in the form of a nanowire. It is during this second deep etching step that MEMS—with at least a 2-order-of-magnitude scale difference - is formed as well. The technique provides a pathway for preserving the lithographic resolution and transforming it into a very high mechanical precision in the assembly of micro- and nanoscales with an extreme topography. Validation of the success of integration is carried out via in situ actuation of MEMS inside an electron microscope loading the nanowire up to its fracture. The technique yields nanowires on the top surface of MEMS, thereby providing ease of access for the purposes of carrying out surface processes such as doping and contact formation as well as in situ observation. As the first study demonstrating such monolithic integration in thick SOI, the work presents a pathway for scaling down to nano for future MEMS combining multiple scales.
Microstructure, smoothening effect, and local defects of alumina sol-gel coatings on ground steel
(2017)
Porous alumina films with thicknesses of a few microns were prepared via a dip-coating technique on steel P92. The coating is shown to protect the steel against massive corrosion, which is typical in the hot reactive environment of coal fired power plants. To mimic real conditions ground steel plates were coated with a boehmite-sol. This leads to an overall smoothing of the formerly rough surface. In the following short annealing step the inner porous construction with worm-like particles consisting of nano-crystallites and amorphous alumina is formed. Due to the simultaneous diffusion of chromium and iron ions out of the bulk steel material into the porous alumina coating, a dense interface with satisfactory adhesion is formed. However, the film exhibits few local defects like cracks or dense alumina nodules caused by steep edges in the ground surface or agglomeration of boehmite-sol components, respectively. Cracks especially have to be avoided. This problem can be overcome so far by slight modifications in the sol preparation process and surface treatment of the substrates. Nevertheless the results demonstrate the potential of sol-gel based alumina coatings as a time- and cost-saving protection type for commercial steel P92.
The present talk serves the routine characterization of the porous structure of unordered anatase NP-fillings by screen printing. Therefore the Focused Ion Beam technique was used to cut a defined volume of material slice per slice of the given material. From each slice electron micrographs are recorded. The won stack of images is than further processed using binarization and segmentation to reconstruct either the mesh of particles or pores. From the calibrated length-scales in the scanning electron microscope it is possible to determine the particular volumes for pore and material.