Abstract: Strain is routinely used in state-of-the-art semiconductor devices in order to improve their electrical performance. Here we present experimental strain measurements obtained by different transmission electron microscopy (TEM) based techniques. Dark field electron holography, nanobeam electron diffraction (NBED) and high angle annular dark field scanning electron microscopy (HAADF STEM) are demonstrated. In this paper we demonstrate the spatial resolution and sensitivity of these different techniques on a simple calibration specimen where the accuracy of the measurement can easily be assessed.
Abstract: Titanium aluminide (TiAl) is a lightweight intermetallic compound with a range of exceptional mid-to-high temperature mechanical properties. These characteristics have the potential to deliver significant weight savings in aero engine components. However, the relatively low ductility of TiAl requires improved understanding of the relationship between manufacturing processes and residual stresses in order to expand the use of such components in service. Previous studies have suggested that stress determination at high spatial resolution is necessary to achieve better insight. The present paper reports progress beyond the current state-of-the-art towards the identification of the near-surface intragranular residual stress state in cast and ground TiAl at a resolution better than 5μm. The semi-destructive ring-core drilling method using Focused Ion Beam (FIB) and Digital Image Correlation (DIC) was used for in-plane residual stress estimation in ten grains at the sample surface. The nature of the locally observed strain reliefs suggests that tensile residual stresses may have been induced in some grains by the unidirectional grinding process applied to the surface.
Abstract: In this study, three different a-C:H:W coatings with predefined hardness values, ranging from 10 up to 16 GPa, were deposited by adjusting bias voltage according to a previously created regression model. For this purpose, the influence of the main process parameters of the used reactive unbalanced magnetron sputtering process on the mechanical properties of the a-C:H:W coating was investigated previously by nanoindentation. For a systematical evaluation of the single effects, parameters were varied according to a central composite design. The three coating variants of this study were investigated in terms of microstructure, mechanical properties and residual stresses. It turned out, that by the use of the regression model, a-C:H:W coatings with tailored mechanical properties can be deposited. Residual stresses were measured by means of focused ion beam milling of a double-slit geometry, which causes the internal stresses to relax, and mapping of the resultant relief strain by digital image correlation. A linear relation between the applied bias voltage and the hardness, the modulus of the coating as well as the determined relief strain was observed. Thus, residual stresses of the coatings increase disproportionately with applied bias voltage. The obtained results can be helpful for tailored coating design and further optimization of a-C:H:W coatings.
Abstract: Oxide dispersive steel is a promising material for next nuclear reactors generation. Performance of this material in nuclear reactor can be modeled by means of irradiation by swift Bi ions, which are typical nuclear fusion products. Radiation damage results in microstructure alternation leading to formation of micro and macro stresses that influence the material performance. The residual stress state of ferrite matrix of the steel is investigated by XRD methodic and dependence on the irradiation dose is analyzed.
Abstract: Palladiums tubular membranes are developed to operate up to 400 °C, for the synthesis of H2 and for the separation of CO2 in Water Gas Shift (WGS) processes and reforming gas of methane [. Palladium has FCC lattice that allows the separation of hydrogen from carbon dioxide through a solution-diffusion mechanism [. To ensure high selectivity in the separation process, the functional Pd layer on the porous substrate of the membranes must have a microstructure with low defects and free from residual stresses [.MicroXRD measurements were performed to evaluate the effect of the stress-relief heat treatment, carried out for different time and temperatures, on the palladium layer. Microstrains were assessed before and after stress-relief by the Williamson-Hall method [. The use of microdiffraction was mandatory considering the tubular shape of membranes. The data were corrected for elastic anisotropy of palladium and the altered Williamson-Hall method was successfully applied.The XRD two-dimensional (2D) images and the integrated spectra collected from the samples allowed to study also the evolution of Pd microstructure and the reduction of micro-stresses due to stress relief. The results of the study allowed to identify the optimal thermal profile for the heat treatment of palladium membranes.
Abstract: A relationship between dislocation density and macro strain was investigated for GLIDCOP, dispersion-strengthened copper with ultra-fine particles of aluminum oxide. The dislocation density was estimated by applying the Warren-Averbach method to a diffraction profile measured using synchrotron radiation.
Abstract: Microstructure and residual stress in AISI316 stainless steels processed via shot peening (SP) and laser peening (LP) were evaluated using X-ray line profile analysis and residual stress measurements. Although both specimens exhibited similar compressive residual stress profiles in the depth direction, the dislocation density in the SP specimen was greater than that in the LP specimen, while the crystallite size in the SP specimen was less than that of the LP specimen. Thus, the variation in the microstructural features in the samples subjected to the two processes differed.
Abstract: The Kossel microdiffraction in a scanning electron microscope allows for local stress determination. This technique has been applied to monitor stress evolution within grains of austenite in the course of martensitic transformation in a shape memory alloy. Kossel diffraction patterns were recorded during in situ tensile straining of Cu-Al-Be alloy. These innovative measurements show large stress heterogeneities between grains, with the stress ratio exceeding two. As martensite variants are stress-induced, shear stress components appear in individual grains of austenite.
Abstract: Kossel microdiffraction is one of a few experimental methods of investigating heterogeneities of elastic stresses within crystallites. With digitally recorded back-reflection Kossel patterns, one can determine absolute lattice parameters, and hence lattice strains and stresses, based on geometry of Kossel lines, but the strain resolution of this approach is limited by finite widths of the lines. A new method is proposed which considerably improves the resolution in cases when the patterns originate from areas with similar lattice orientations. The method is based on determination of differences between pattern geometries: lattice strains are calculated from mutual shifts of intensity profiles of Kossel lines. The strain accuracy of this profile-based approach was estimated. It is demonstrated that the limit of strain resolution reaches a few parts per hundred thousand, i.e., it is nearly one order of magnitude better than that of the conventional Kossel-based lattice parameter refinement. This improvement concerns the critical range of lattice strain, and it constitutes a qualitative leap in resolution. The paper describes main aspects of the new approach and strain resolution tests.